Sarcosine → HCID 22662727、化合物

HRID 1060534

反応式

HRID 1060534 の反応式
[OH-].[Na+].Cl[S:4]([C:7]1[C:11]2[CH:12]=[CH:13][CH:14]=[CH:15][C:10]=2[S:9][CH:8]=1)(=[O:6])=[O:5].[NH:16]([CH2:18][C:19]([OH:21])=[O:20])[CH3:17].C1(C)C=CC=CC=1>O>[S:9]1[C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][C:11]=2[C:7]([S:4]([N:16]([CH2:18][C:19]([OH:21])=[O:20])[CH3:17])(=[O:6])=[O:5])=[CH:8]1

参加物

6

反応物 4

HCID 1088SarcosineHCID 1140TolueneHCID 14798Sodium HydroxideHCID 27763401-Benzothiophene-3-sulfonyl chloride

生成物 1

HCID 22662727HCID 22662727、化合物

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
60 °C

実験手順

6 g of NaOH, 23.27 g of 3-chlorosulphonyl-benzothiophene and 13.36 g of sarcosine are added to a mixture of 200 ml of toluene and 200 ml of water and stirred for 6.5 hours at 60° C. For working up, the aqueous phase is separated off and the organic phase is extracted with 100 ml of 2 N NaOH solution. The combined aqueous phases are acidified with conc. HCl and then extracted twice with 300 ml of ethyl acetate. After washing with saturated aqueous saline solution and drying over magnesium sulphate the organic phase is concentrated by evaporation. The crude product obtained is recrystallised from 100 ml of dichloroethane. Yield: 13.14 g. M.p.: 139-140° C.

後処理

  1. customthe aqueous phase is separated off
  2. extractionthe organic phase is extracted with 100 ml of 2 N NaOH solution
  3. extractionextracted twice with 300 ml of ethyl acetate
  4. washAfter washing with saturated aqueous saline solution
  5. dry with materialdrying over magnesium sulphate the organic phase
  6. concentrationis concentrated by evaporation

出典と根拠

ORDレコード
ord-e63a3461ef814ffcb95ef53bca701930
出典データセット
uspto-grants-2003_02
特許番号
US06525045B2

関連ノート

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