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HCID 12764242、化合物 → 1-(3-Benzoylsulfanyl-propionyl)-2,3-dihydro-1H-indole-2-carboxylic acid

HRID 1262906
ノート
印刷プレビュー

反応式

HRID 1262906 の反応式
[O:1]=[C:2]([N:5]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7][CH:6]1[C:14]([OH:16])=[O:15])[CH:3]=[CH2:4].[C:17]([OH:25])(=[S:24])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>C(Cl)Cl>[C:17]([S:24][CH2:4][CH2:3][C:2]([N:5]1[C:13]2[C:8](=[CH:9][CH:10]=[CH:11][CH:12]=2)[CH2:7][CH:6]1[C:14]([OH:16])=[O:15])=[O:1])(=[O:25])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 12764242HCID 12764242、化合物HCID 178526132HCID 178526132、化合物

生成物 1

HCID 127642431-(3-Benzoylsulfanyl-propionyl)-2,3-dihydro-1H-indole-2-carboxylic acid

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a stirring mixture of 2,3-dihydro-1-(1-oxo-2-propenyl)-1H-indole-2-carboxylic acid (6.52 g.) and methylene chloride 160 ml.) was added dropwise thiobenzoic acid (95%, 4.36 g.) dissolved in a small amount of methylene chloride. During the addition, the reaction mixture was chilled in ice. The ice bath was removed in 10 minutes after the completion of the addition, but the stirring was continued for 1 hour. The reaction mixture was then immersed in an oil bath maintained at 80° for 2.5 hours. The reaction mixture was concentrated on a rotary evaporator under reduced pressure to ca. 30 ml., and kept in a refrigerator for 1 day. A precipitate was collected on a filter and washed with methylene chloride to give the titled compound which melted at 173°-175°, and weighed 11.0 g.

後処理

  1. additionDuring the addition
  2. temperaturethe reaction mixture was chilled in ice
  3. customThe ice bath was removed in 10 minutes
  4. additionafter the completion of the addition
  5. customThe reaction mixture was then immersed in an oil bath
  6. temperaturemaintained at 80° for 2.5 hours
  7. concentrationThe reaction mixture was concentrated on a rotary evaporator under reduced pressure to ca. 30 ml
  8. wait, and kept in a refrigerator for 1 day
  9. customA precipitate was collected on
  10. filtrationa filter
  11. washwashed with methylene chloride

出典と根拠

ORDレコード
ord-40bdc9c650464706961d351bd4e16c82
出典データセット
uspto-grants-1984_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04454292

反応ノート

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