SU165699A1 - - Google Patents
Info
- Publication number
- SU165699A1 SU165699A1 SU744496A SU744496A SU165699A1 SU 165699 A1 SU165699 A1 SU 165699A1 SU 744496 A SU744496 A SU 744496A SU 744496 A SU744496 A SU 744496A SU 165699 A1 SU165699 A1 SU 165699A1
- Authority
- SU
- USSR - Soviet Union
- Prior art keywords
- pyridine
- mol
- calculated
- found
- cyanohydrin
- Prior art date
Links
- JUJWROOIHBZHMG-UHFFFAOYSA-N pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 description 6
- 150000002576 ketones Chemical class 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000000875 corresponding Effects 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 150000003871 sulfonates Chemical class 0.000 description 2
- FHUDAMLDXFJHJE-UHFFFAOYSA-N 1,1,1-trifluoropropan-2-one Chemical compound CC(=O)C(F)(F)F FHUDAMLDXFJHJE-UHFFFAOYSA-N 0.000 description 1
- CSKNSYBAZOQPLR-UHFFFAOYSA-N Benzenesulfonyl chloride Chemical compound ClS(=O)(=O)C1=CC=CC=C1 CSKNSYBAZOQPLR-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000012044 organic layer Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L sulfate Chemical class [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- XTHPWXDJESJLNJ-UHFFFAOYSA-N sulfurochloridic acid Chemical compound OS(Cl)(=O)=O XTHPWXDJESJLNJ-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Description
До насто щего времени не был известен снособ получени сульфонатов кетонциангидринов .Until now, the method for the preparation of ketoncyanohydrin sulfonates has not been known.
Предлагаемый снособ состоит в том, что кетонциаигидрин подвергают взаимодействию с эквимолекул рной смесью соответствующего сульфохлорида и пиридина. Это ноззол ет получать сульфоиаты кетонциангидринов .The proposed removal procedure is that the ketone cyahydrin is reacted with an equimolecular mixture of the corresponding sulfochloride and pyridine. It is not necessary to obtain ketone cyanohydrin sulfoates.
При осуществлении способа реакцию провод т при темнературе 15-20°С.In the process, the reaction is carried out at a temperature of 15-20 ° C.
Пример. К смеси анетонциангидрина (0,5 моль и пиридина (0,55 моль) нрибавл ют при охлаждении и перемеишвапии бензолсульфохлорид (0,55 моль). Затем реакционную смесь выдержива от нри ко.мнатной те.мпературе в течение нескольких часов до выпадени кристаллов.Example. To a mixture of anethocyanhydrin (0.5 mol and pyridine (0.55 mol), benzenesulfonyl chloride (0.55 mol) was added under cooling and stirring. The reaction mixture was then kept from room temperature for several hours until the crystals precipitated.
Реакционную массу нейтрализуют нри охлаждении разбавленной сол ной кислотойи промывают водой.The reaction mass is neutralized by cooling with dilute hydrochloric acid and washed with water.
Вес органического сло (сульфоиат-сырец) G6,75 г (60%). Сырец разгон ют под вакуумом (11 The weight of the organic layer (sulfoiat raw) is G6.75 g (60%). The raw material is distilled under vacuum (11
ММ Hg) MM Hg)
и получают вещество с т. I мм рт. ст.); пи 1,5071; -130°С ( кип, 129рт .and receive substance with t. I mm of mercury. Art.); pi 1.5071; -130 ° С (kip, 129tr.
2°2 °
1,2205; MR D 54,45 (найдено дл 1.2205; MR D 54.45 (found for
С4 CioHiiNOaS) и 54,13 (вычислено).C4 CioHiiNOaS) and 54.13 (calculated).
Найдено, %: С 53,52; 53,46; И 4,47, 4.66; N5,47, 5,74; S 13,27, 13,06. Вычислено; С 53,40; Н 4,88; N 6,22; S 14,43. Диалогично получают бензолсульфопат 1,1,1-трифторацетонциангидрина с выходом 52% от теоретического. Т. кип.Found,%: C 53.52; 53.46; And 4.47, 4.66; N5.47, 5.74; S 13.27, 13.06. Calculated; C 53.40; H 4.88; N 6.22; S 14.43. Dialogically receive benzenesulfate 1,1,1-trifluoroacetone cyanohydrin with a yield of 52% of the theoretical. T. Kip.
2020
2020
1,4622; d 1,3715.1.4622; d 1.3715.
(1 мм рт. ст.); t.,j 1,-tui, li 4(1 mm Hg. Art.); t., j 1, -tui, li 4
87°С87 ° C
Найдено, .%: С 43,13, 43,07; Н 2,61, 2,94; N 5,59, 5,48: S 10,84, 11,25; CloHsNOjSF;,. Вычислено; С 43,11; Н 2,87; N 5,02; S 11,48.Found,%: C 43.13, 43.07; H 2.61, 2.94; N 5.59, 5.48: S 10.84, 11.25; CloHsNOjSF;,. Calculated; C 43.11; H 2.87; N 5.02; S 11.48.
Предмет изобретени Subject invention
Снособ получени сульфонатов кетонциангидринов , о т л и ч а ю щ и и с тем, что кетон0 циангидрин подвергают взаимодействию с эквимолекул рной смесью соответствующего сульфохлорида и пиридина.A process for the preparation of keton cyanohydrin sulfonates, which is such that ketone cyanhydrin is reacted with an equimolecular mixture of the corresponding sulfonic chloride and pyridine.
Publications (1)
Publication Number | Publication Date |
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SU165699A1 true SU165699A1 (en) |
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