Lithium Hydroxide → 2-(N-(4-bromobenzenesulphonyl)-N-methylaminomethyl)thiazole-4-carboxylic acid

HRID 901961노트

반응식

HRID 901961 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:11]([CH2:13][C:14]2[S:15][CH:16]=[C:17]([C:19]([O:21]CC)=[O:20])[N:18]=2)[CH3:12])(=[O:10])=[O:9])=[CH:4][CH:3]=1.[OH-].[Li+]>O1CCOCC1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:11]([CH2:13][C:14]2[S:15][CH:16]=[C:17]([C:19]([OH:21])=[O:20])[N:18]=2)[CH3:12])(=[O:10])=[O:9])=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 69206070HCID 69206070, 화합물

생성물 1

HCID 692074192-(N-(4-bromobenzenesulphonyl)-N-methylaminomethyl)thiazole-4-carboxylic acid수율 95%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
50 °C

실험 절차

Ethyl 2-(N-(4-bromobenzenesulphonyl)-N-methylaminomethyl)thiazole-4-carboxylate (2.19, 5.2 mmol) was added to mixture of 1N lithium hydroxide solution (10 ml, 10 mmol) and dioxan (20 ml) and heated to 50° C. until a solution was obtained. The mixture was stirred at room temperature for a further 3 days. The mixture was evaporated, taken up in EtOAc and acidified with 1N potassium hydrogen sulphate solution. The phases were separated and the organic phase washed with water and brine, dried and reduced to afford 2-(N-(4-bromobenzenesulphonyl)-N-methylaminomethyl)thiazole-4-carboxylic acid (1.86 g, 95%) as a white solid.

후처리

  1. customwas obtained
  2. customThe mixture was evaporated
  3. customThe phases were separated
  4. washthe organic phase washed with water and brine
  5. customdried

출처 및 근거

ORD 기록
ord-adcc4646ff894c33bd5e5edf168701bd
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07365065B2

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