Sodium Acetate → 4-Chloroacetamidothiazole

HRID 1413214노트

반응식

HRID 1413214 반응식
Br[C:2]1[S:3][CH:4]=[C:5]([NH:7][C:8](=[O:11])[CH2:9][Cl:10])[N:6]=1.C([O-])(=O)C.[Na+].[H][H]>CO.[Pd]>[Cl:10][CH2:9][C:8]([NH:7][C:5]1[N:6]=[CH:2][S:3][CH:4]=1)=[O:11]

참가 물질

6

반응물 3

HCID 517045Sodium AcetateHCID 202940332-Bromo-4-chloroacetamidothiazoleHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 202940394-Chloroacetamidothiazole수율 57.9%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

A solution of 2-bromo-4-chloroacetamidothiazole (4 g) and sodium acetate (1.15 g) in methanol (100 ml) was hydrogenated at atmospheric pressure over 10% Pd/C catalyst (1 g) until theoretical uptake of hydrogen had occurred. The catalyst was removed by filtration and washed with methanol and the extracts evaporated to dryness in vacuo. The residue was recrystallised twice from carbon tetrachloride to give the title compound (1.6 g) m.p. 115°-119° C. (Found: C, 33.7; H, 2.9; N, 15.5. C5H5ClN2OS requires C, 34.0; H, 2.9; N, 15.8%).

후처리

  1. customThe catalyst was removed by filtration
  2. washwashed with methanol
  3. customthe extracts evaporated to dryness in vacuo
  4. customThe residue was recrystallised twice from carbon tetrachloride

출처 및 근거

ORD 기록
ord-fe2c8561a9974687921e79e9c14c945e
출처 데이터셋
uspto-grants-1981_02
특허 번호
US04249012

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