JPS5446722A - Novel preparation of s-2-(3-aminopropyl-amino) ethyldihydrogenphosphorothioate monohydrate crystal - Google Patents

Novel preparation of s-2-(3-aminopropyl-amino) ethyldihydrogenphosphorothioate monohydrate crystal

Info

Publication number
JPS5446722A
JPS5446722A JP11360177A JP11360177A JPS5446722A JP S5446722 A JPS5446722 A JP S5446722A JP 11360177 A JP11360177 A JP 11360177A JP 11360177 A JP11360177 A JP 11360177A JP S5446722 A JPS5446722 A JP S5446722A
Authority
JP
Japan
Prior art keywords
crystal
ethyldihydrogenphosphorothioate
ethanol
aminopropylamino
monohydrate crystal
Prior art date
Legal status (The legal status 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 status listed.)
Granted
Application number
JP11360177A
Other languages
Japanese (ja)
Other versions
JPS6041676B2 (en
Inventor
Kiyoshi Okazaki
Hiromitsu Kawada
Mutsuo Takashima
Hidemi Shimizu
Takeshi Sato
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yamanouchi Pharmaceutical Co Ltd
Original Assignee
Yamanouchi Pharmaceutical Co Ltd
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 Yamanouchi Pharmaceutical Co Ltd filed Critical Yamanouchi Pharmaceutical Co Ltd
Priority to JP11360177A priority Critical patent/JPS6041676B2/en
Publication of JPS5446722A publication Critical patent/JPS5446722A/en
Publication of JPS6041676B2 publication Critical patent/JPS6041676B2/en
Expired legal-status Critical Current

Links

Abstract

PURPOSE: To obtain the titled compound free from methanol, by suspending a polyhydrate crystal of S-2-(3-aminopropylamino) ethyldihydrogenphosphorothioate in ethanol, and by treating the suspension at a specific temperaure to transform the thioate into a monohydrate crystal.
CONSTITUTION: The titled compound is prepared by anyone of the following three methods: (A) A suspension of a polyhydrate crystal of S-2-(3-aminopropylamino)- ethyldihydrogenphosphorothioate in ethanol is treated in an ice bath or at a temperature of 60°C or below to transform the crystal into a monohydrate crystal to give the desired compound (B) A polyol containing or free from ethanol which is usually not used as a crystallization solvent is added to an aqueous solution of crude S-2-(3-aminopropylamino) ethyldihydroenphosphorothioate. (C) The aqueous solution is added to individual ethanol or polyol, or their mixture to crystallize the objective compound in a high yield.
USE: Radiation protectives.
COPYRIGHT: (C)1979,JPO&Japio
JP11360177A 1977-09-21 1977-09-21 New method for producing S-2-(3-aminopropylamino)ethyldihydrodiene phosphorothioate monohydrate crystals Expired JPS6041676B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP11360177A JPS6041676B2 (en) 1977-09-21 1977-09-21 New method for producing S-2-(3-aminopropylamino)ethyldihydrodiene phosphorothioate monohydrate crystals

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP11360177A JPS6041676B2 (en) 1977-09-21 1977-09-21 New method for producing S-2-(3-aminopropylamino)ethyldihydrodiene phosphorothioate monohydrate crystals

Publications (2)

Publication Number Publication Date
JPS5446722A true JPS5446722A (en) 1979-04-12
JPS6041676B2 JPS6041676B2 (en) 1985-09-18

Family

ID=14616338

Family Applications (1)

Application Number Title Priority Date Filing Date
JP11360177A Expired JPS6041676B2 (en) 1977-09-21 1977-09-21 New method for producing S-2-(3-aminopropylamino)ethyldihydrodiene phosphorothioate monohydrate crystals

Country Status (1)

Country Link
JP (1) JPS6041676B2 (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5591731A (en) * 1992-07-31 1997-01-07 U.S. Bioscience, Inc. Crystalline amifostine compositions
US6384259B1 (en) 1998-11-16 2002-05-07 Medimmune Oncology, Inc. Stable amorphous amifostine compositions and dosage form
US6407278B2 (en) 1998-11-16 2002-06-18 Medimmune Oncology, Inc. Stable amorphous amifostine compositions and methods for the preparation and use of the same
EP1243272A2 (en) 1992-07-31 2002-09-25 Medimmune Oncology, Inc. Crystalline amifostine compositions and methods for the preparation and use of same
US7629333B2 (en) 2002-03-29 2009-12-08 Medimmune, Llc Stable amorphous amifostine compositions and methods for the preparation and use of same

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5591731A (en) * 1992-07-31 1997-01-07 U.S. Bioscience, Inc. Crystalline amifostine compositions
EP1243272A2 (en) 1992-07-31 2002-09-25 Medimmune Oncology, Inc. Crystalline amifostine compositions and methods for the preparation and use of same
EP1243272A3 (en) * 1992-07-31 2003-01-22 Medimmune Oncology, Inc. Crystalline amifostine compositions and methods for the preparation and use of same
EP1764103A3 (en) * 1992-07-31 2011-08-24 Medimmune Oncology, Inc. Crystalline amifostine compositions and methods for the preparation and use of same
US6384259B1 (en) 1998-11-16 2002-05-07 Medimmune Oncology, Inc. Stable amorphous amifostine compositions and dosage form
US6407278B2 (en) 1998-11-16 2002-06-18 Medimmune Oncology, Inc. Stable amorphous amifostine compositions and methods for the preparation and use of the same
US6841545B2 (en) 1998-11-16 2005-01-11 Medimmune Oncology, Inc. Stable amorphous amifostine compositions and methods for the preparation of same
US7629333B2 (en) 2002-03-29 2009-12-08 Medimmune, Llc Stable amorphous amifostine compositions and methods for the preparation and use of same

Also Published As

Publication number Publication date
JPS6041676B2 (en) 1985-09-18

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