Sarcosine → HCID 22662727, 화합물

HRID 1060534

반응식

HRID 1060534 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

HCID 22662727HCID 22662727, 화합물

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
60 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e63a3461ef814ffcb95ef53bca701930
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06525045B2

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