Potassium Hydroxide → 6-Mercapto-8-methylthiooctanoic acid

HRID 247184노트

반응식

HRID 247184 반응식
C([O:3][C:4](=[S:17])[CH2:5][CH2:6][CH2:7][CH2:8][CH:9]([S:13]C(=O)C)[CH2:10][CH2:11][CH3:12])C.[OH-].[K+]>CO.O>[SH:13][CH:9]([CH2:10][CH2:11][CH3:12])[CH2:8][CH2:7][CH2:6][CH2:5][C:4]([OH:3])=[S:17]

참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 53988615HCID 53988615, 화합물

생성물 1

HCID 1784549696-Mercapto-8-methylthiooctanoic acid

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

11.9 grams (40.7 mmoles) of 6-acetylthio-8-methylthiooctanoic acid ethyl ester (XI) were added to a solution of 7.5 grams (133.7 mmoles) of potassium hydroxide in 100 ml of methanol and 5 ml of water and the mixture heated at reflux for 10 hours under a cover of nitrogen. After a further 10 hours at room temperature the solvent was removed in a vacuum, the residue taken up on 100 ml of 3N hydrochloric acid and extracted three times, each time with 100 ml of ethyl acetate. After drying the combined extracts with magnesium sulfate the solvent was removed in a vacuum. The short path distillation of the residue gave 7.1 grams (78% of theory) of 6-mercapto-8-methylthiooctanoic acidas a pale yellow oil having a boiling point of 150° C. to 170° C. at 0.5 mbar.

후처리

  1. temperaturethe mixture heated
  2. temperatureat reflux for 10 hours under a cover of nitrogen
  3. customAfter a further 10 hours at room temperature the solvent was removed in a vacuum
  4. extractionextracted three times
  5. dry with materialAfter drying the combined extracts with magnesium sulfate the solvent
  6. customwas removed in a vacuum
  7. distillationThe short path distillation of the residue
  8. customgave 7.1 grams (78% of theory) of 6-mercapto-8-methylthiooctanoic acidas a pale yellow oil

출처 및 근거

ORD 기록
ord-ae6888ac8a8b40b78ba7df08fa4d9cd4
출처 데이터셋
uspto-grants-1987_11
특허 번호
US04705867

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