KR830009012A - Method for Purifying Para-Tosyl Chloride - Google Patents

Method for Purifying Para-Tosyl Chloride Download PDF

Info

Publication number
KR830009012A
KR830009012A KR1019820001071A KR820001071A KR830009012A KR 830009012 A KR830009012 A KR 830009012A KR 1019820001071 A KR1019820001071 A KR 1019820001071A KR 820001071 A KR820001071 A KR 820001071A KR 830009012 A KR830009012 A KR 830009012A
Authority
KR
South Korea
Prior art keywords
tosyl chloride
para
toluene
chloride
dissolution
Prior art date
Application number
KR1019820001071A
Other languages
Korean (ko)
Other versions
KR840002200B1 (en
Inventor
윤창구
한승희
김도현
Original Assignee
임관
한국과학기술원
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 임관, 한국과학기술원 filed Critical 임관
Priority to KR8201071A priority Critical patent/KR840002200B1/en
Priority to JP57224824A priority patent/JPS5932461B2/en
Publication of KR830009012A publication Critical patent/KR830009012A/en
Application granted granted Critical
Publication of KR840002200B1 publication Critical patent/KR840002200B1/en

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C17/00—Preparation of halogenated hydrocarbons
    • C07C17/38—Separation; Purification; Stabilisation; Use of additives

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

내용 없음No content

Description

파라-토 실클로라이드의 정제방법Method for Purifying Para-Tosyl Chloride

본 내용은 요부공개 건이므로 전문내용을 수록하지 않았음Since this is an open matter, no full text was included.

도 1은 온도에 따르는 톨루엔중의 파라토실클로라이드의 용해도 곡설이며,1 is a solubility curve of paratosyl chloride in toluene with temperature,

도 2은 위의 정제방법의 공정도이다.2 is a process chart of the above purification method.

Claims (6)

톨루엔과 염화술폰산을 반응시켜 오르토-토실클로라이드를 제조할 때에 부생되는 파리-토실클로라이드를 회수, 정제함에 있어서, 반응공정(1), 희석공정(2), 용해. 추출공정(6), 재결정공정(8) 및 분리공정(9)으로 이루어지며 별도로 용제를 회수할 필요없이 정제 모액에 함유된 파리-토실클로라이드와 오르토-토실클로라이드를 회수하고 톨루엔은 오르토-토실클로라이드와 파라-토실클로라이드의 제조원료로 사용함을 특징으로 하는 파라-토실클로라이드의 회수. 정제방법.Reaction step (1), dilution step (2), dissolution in recovering and purifying fly-tosyl chloride which is a by-product when toluene is reacted with sulfonic acid to produce ortho-tosyl chloride. Extraction process (6), recrystallization process (8), and separation process (9). It is possible to recover the fly-tosyl chloride and ortho-tosyl chloride contained in the purified mother liquor without separately recovering the solvent, and toluene is ortho-tosyl chloride. Recovery of para-tosyl chloride, characterized in that used as a raw material for the preparation of para-tosyl chloride. Purification method. 제1항에 있어서, 반응공정(1) 이라함은 톨루엔에 대한 염화술폰산의 몰비가 1-5로 구성된 혼합액을 -15-25℃에서 30분-4시간 동안 염화술폰화함을 특징으로 하는 공정.The process according to claim 1, wherein the reaction step (1) is characterized in that the mixture of sulfonate to toluene has a molar ratio of 1-5, which is sulfonated at -15-25 ° C for 30 minutes-4 hours. 제1항에 있어서, 희석공정(2)이라 함은 미반응 염화술폰산을 파괴하기 위하여 물을 첨가하여 수용액층이 5-90%(무게)의 황산이 되는 것을 특징으로하는 공정.The process according to claim 1, wherein the dilution step (2) is characterized in that the aqueous solution layer is 5-90% (weight) sulfuric acid by adding water to destroy unreacted sulfonic acid chloride. 제1항에 있어서, 용해. 추출공정(6) 이라함은 분리공정(3)과 세척공정(4)으로 부터 얻어진 조 파라-토실클로라이드와 조파라-토실클로라이드 1g에 대하여 톨루엔 0.2-5㎖와 톨루엔의 0-5배(부피)의 물을 혼합하여 20-40℃에서 용해. 추출시킴을 특징으로 하는 공정.The dissolution according to claim 1, wherein the dissolution. Extraction process (6) means 0-5 times (volume of 0.2-5 ml of toluene and 1 toluene with respect to 1 g of crude para-tosylchloride and crude para-tosyl chloride obtained from separation process (3) and washing process (4). ) Is mixed and dissolved at 20-40 ℃. Process characterized by extraction. 제1항에 있어서, 재결정공정(8) 이라함은 정치. 탈수공정(7)에서 탈수된 파라-토실클로라이드 함유유기용액을 -5-30℃로 냉각하여 파라-토실클로라이드를 재결정화 함을 특징으로 하는 공정 .The process according to claim 1, wherein the recrystallization process (8) is stationary. The para-tosyl chloride-containing organic solution dehydrated in the dehydration step (7) is cooled to -5-30 ° C. to recrystallize the para-tosyl chloride. 제1항에 있어서, 분리공정(9)이라함은 재결정된 정재 파라-토실클로라이드를 제조함과 동시에 정제모액을 반응공정(1) 또는 용해. 추출공정(6)으로 이송시킴을 특징으로 하는 공정.The process according to claim 1, wherein the separation step (9) is to prepare recrystallized refined para-tosylchloride and simultaneously purify the purified mother liquor. Characterized in that the transfer to the extraction process (6). ※ 참고사항 : 최초출원 내용에 의하여 공개하는 것임.※ Note: The disclosure is based on the initial application.
KR8201071A 1982-03-12 1982-03-12 Purification of p-tosyl chloride KR840002200B1 (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
KR8201071A KR840002200B1 (en) 1982-03-12 1982-03-12 Purification of p-tosyl chloride
JP57224824A JPS5932461B2 (en) 1982-03-12 1982-12-21 Method for purifying p-toluenesulfonic acid chloride

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
KR8201071A KR840002200B1 (en) 1982-03-12 1982-03-12 Purification of p-tosyl chloride

Publications (2)

Publication Number Publication Date
KR830009012A true KR830009012A (en) 1983-12-17
KR840002200B1 KR840002200B1 (en) 1984-11-28

Family

ID=19224161

Family Applications (1)

Application Number Title Priority Date Filing Date
KR8201071A KR840002200B1 (en) 1982-03-12 1982-03-12 Purification of p-tosyl chloride

Country Status (2)

Country Link
JP (1) JPS5932461B2 (en)
KR (1) KR840002200B1 (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6153093A (en) * 1984-08-22 1986-03-15 江本紙工品株式会社 Method of book-binding album, etc.
US5252759A (en) * 1993-01-29 1993-10-12 Arco Chemical Technology, L.P. Process for producing optically active epoxy alcohol derivatives

Also Published As

Publication number Publication date
KR840002200B1 (en) 1984-11-28
JPS5932461B2 (en) 1984-08-09
JPS58162570A (en) 1983-09-27

Similar Documents

Publication Publication Date Title
US4162270A (en) Process for producing 4,4'-dihydroxydiphenylsulfone of high purity
GB946322A (en) Process for purifying 4,4 dihydroxydiphenylpropane 2,2
SU496730A3 (en) The method of obtaining derivatives of isoindoline or their salts
US4113974A (en) Process for purifying impure diphenols
US4820831A (en) Process for preparing 4,4'-dihydroxydiphenyl sulfone having high purity
KR870005949A (en) Recrystallization Method Of Bisphenol A
KR830009012A (en) Method for Purifying Para-Tosyl Chloride
US4012451A (en) Process for the separation of 4,4'-dichlorodiphenylsulfone
KR960007528A (en) Method of preparing dinitrotoluene
US3108137A (en) Production of organic sulfonyl chlorides
US4420642A (en) Selective removal and recovery of catechol mixed with 2-methallyloxyphenol
US4145349A (en) Process for the production of saccharine
KR880000389A (en) Separation method of monohydrate of L-cysteine hydrochloride
US4065477A (en) Process for preparing highly pure 1-nitroanthraquinone
US3115501A (en) Sultone manufacture
CN107417560B (en) Method for synthesizing tiramide hydrochloride
SU1114677A1 (en) Process for preparing benzo-2,1,3-thiadiazole
US4242275A (en) Process for the preparation of isomer-free toluene-4-sulfonic acid
US2409806A (en) Synthesis of nicotinic compounds
KR840002241A (en) Process of making a laxative from senna
US4701567A (en) Process for producing 6,6'-dihydroxy-3,3,3',3'-tetramethyl-1,1'-spirobiindane
BR9804440A (en) Adiabatic process for the production of dinitrotoluene
US2748161A (en) Method of forming phthalaldehydic acid from pentachloroxylene
SU1133254A1 (en) Process for purifying benzo(b)thiophene and naphthalene from naphthalene cut
JP2798293B2 (en) How to recover phenols