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

HRID 745612ノート

反応式

HRID 745612 の反応式
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

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-a1796d3f5e99487dabf1310fc99350ba
出典データセット
uspto-grants-1986_07
特許番号
US04599357

反応ノート

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