Triethylamine → 1-(3-Benzoylthio-2-methylpropanoyl)-3,3-dimethylindoline-2-carboxylic acid

HRID 745612노트

반응식

HRID 745612 반응식
Cl.[CH3:2][C:3]1([CH3:15])[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[NH:5][CH:4]1[C:12]([OH:14])=[O:13].C(N(CC)CC)C.[C:23]([S:31][CH2:32][CH:33]([CH3:37])[C:34](Cl)=[O:35])(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1>C(Cl)Cl>[C:23]([S:31][CH2:32][CH:33]([CH3:37])[C:34]([N:5]1[C:6]2[C:11](=[CH:10][CH:9]=[CH:8][CH:7]=2)[C:3]([CH3:15])([CH3:2])[CH:4]1[C:12]([OH:14])=[O:13])=[O:35])(=[O:30])[C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 12878433(1)-S-(3-Chloro-2-methyl-3-oxopropyl) benzenecarbothioateHCID 704701543,3-dimethyl-2,3-dihydro-1H-indole-2-carboxylic acid hydrochloride

생성물 1

HCID 233138471-(3-Benzoylthio-2-methylpropanoyl)-3,3-dimethylindoline-2-carboxylic acid

시약·촉매·용매 1

HCID 6344Dichloromethane용매2회

실험 절차

To the suspension of 1.0 g of 3,3-dimethylindoline-2-carboxylic acid hydrochloride in 25 ml of methylene chloride, 1.33 g of triethylamine are added and the resulting solution cooled to -10°. The solution of 1.065 g of 3-benzoylthio-2-methylpropanoyl chloride in 5 ml of methylene chloride is added dropwise and the mixture stirred at -5° for 1 hour, and then at room temperature for 2 hours. It is evaporated, 10 ml of 3N hydrochloric acid are added to the residue and the mixture is extracted with methylene chloride. The extract is dried and evaporated, to give the 1-(3-benzoylthio-2-methylpropanoyl)-3,3-dimethylindoline-2-carboxylic acid.

후처리

  1. additionare added
  2. temperaturethe resulting solution cooled to -10°
  3. waitat room temperature for 2 hours
  4. customIt is evaporated
  5. addition10 ml of 3N hydrochloric acid are added to the residue
  6. extractionthe mixture is extracted with methylene chloride
  7. customThe extract is dried
  8. customevaporated

출처 및 근거

ORD 기록
ord-a1796d3f5e99487dabf1310fc99350ba
출처 데이터셋
uspto-grants-1986_07
특허 번호
US04599357

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