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Hydrochloric Acid → 1-(3-Acetylthiopropanoyl)-3,3-dimethylindoline-2-carboxylic acid

HRID 745606
ノート
印刷プレビュー

反応式

HRID 745606 の反応式
C(N(CC)CC)C.Cl.[CH3:9][C:10]1([CH3:22])[C:18]2[C:13](=[CH:14][CH:15]=[CH:16][CH:17]=2)[NH:12][CH:11]1[C:19]([OH:21])=[O:20].[C:23]([S:26][CH2:27][CH2:28][C:29](Cl)=[O:30])(=[O:25])[CH3:24].Cl>C(Cl)Cl>[C:23]([S:26][CH2:27][CH2:28][C:29]([N:12]1[C:13]2[C:18](=[CH:17][CH:16]=[CH:15][CH:14]=2)[C:10]([CH3:22])([CH3:9])[CH:11]1[C:19]([OH:21])=[O:20])=[O:30])(=[O:25])[CH3:24]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8471TriethylamineHCID 129431223-(Acetylsulfanyl)propanoyl chlorideHCID 704701543,3-dimethyl-2,3-dihydro-1H-indole-2-carboxylic acid hydrochloride

生成物 1

HCID 233138381-(3-Acetylthiopropanoyl)-3,3-dimethylindoline-2-carboxylic acid

試薬・触媒・溶媒 1

HCID 6344
Dichloromethane
溶媒
2 回

実験手順

0.93 g of triethylamine are added to the suspension of 0.7 g of 3,3-dimethylindoline-2-carboxylic acid hydrochloride in 20 ml of methylene chloride and the resulting solution is cooled to -10°. The solution of 0.51 g of 3-acetylthiopropanoyl chloride in 5 ml of methylene chloride is added dropwise and the mixture stirred at -5° to -10° for 1 hour and at room temperature for 3 hours. It is cooled to 0° and treated with 10 ml of 3N hydrochloric acid. The organic layer is separated and the aqueous solution further extracted with methylene chloride. The combined methylene chloride solutions are dried and evaporated, to give the 1-(3-acetylthiopropanoyl)-3,3-dimethylindoline-2-carboxylic acid as a foam.

後処理

  1. temperaturethe resulting solution is cooled to -10°
  2. temperatureIt is cooled to 0°
  3. customThe organic layer is separated
  4. extractionthe aqueous solution further extracted with methylene chloride
  5. dry with materialThe combined methylene chloride solutions are dried
  6. customevaporated

出典と根拠

ORDレコード
ord-fb23bb495720428daa47716788fc5e74
出典データセット
uspto-grants-1986_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04599357

反応ノート

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