Hydrochloric Acid → HCID 178443546, 화합물

HRID 1089398노트

반응식

HRID 1089398 반응식
[CH2:1]([SH:8])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Na].C([O:12][C:13](=[S:23])[CH2:14][CH2:15][CH2:16][CH2:17][CH:18](Cl)[CH2:19][CH2:20][CH3:21])C.[OH-].[K+].Cl>O>[CH2:1]([S:8][CH:18]([CH2:19][CH2:20][CH3:21])[CH2:17][CH2:16][CH2:15][CH2:14][C:13]([OH:12])=[S:23])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 7509Benzyl mercaptanHCID 14797Potassium HydroxideHCID 5360545SodiumHCID 536593926-Chloro-8-methylthiooctanoic acid ethyl ester

생성물 1

HCID 178443546HCID 178443546, 화합물수율 104.9%

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

12.4 grams (0.1 mole) of benzyl mercaptan were added to a solution of 2.3 grams of sodium in 75 ml of water free ethanol (corresponding to 0.1 mole of sodium ethanolate) and the mixture stirred for 0.5 hour at +10° C. Thereupon there were added 22.72 grams (0.09 mole) of 6-chloro-8-methylthiooctanoic acid ethyl ester (X) and the mixture heated for 20 hours at reflux. To the cooled reaction mixture there were added 11.2 grams (0.17 mole) of potassium hydroxide and stirring was carried out for 20 hours at room temperature. After addition of 500 ml of water the mixture was acidified with dilute hydrochloric acid, extracted with dichloromethane, the combined extracts washed with saturated aqueous sodium chloride solution and dried with sodium sulfate. By distilling off the solvent in a vacuum there were obtained 28.0 grams (96% of theory) of crude 6-benzylthio-8-methylthiooctanoic acid.

후처리

  1. temperaturethe mixture heated for 20 hours
  2. temperatureat reflux
  3. customTo the cooled reaction mixture there
  4. stirringstirring
  5. waitwas carried out for 20 hours at room temperature
  6. extractionextracted with dichloromethane
  7. washthe combined extracts washed with saturated aqueous sodium chloride solution
  8. dry with materialdried with sodium sulfate
  9. distillationBy distilling off the solvent in a vacuum there

출처 및 근거

ORD 기록
ord-d5113101b31f45a8836068f3cd75bb7f
출처 데이터셋
uspto-grants-1990_10
특허 번호
US04966732

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