Sodium Acetate → 4-Chloroacetamidothiazole

HRID 1413214ノート

反応式

HRID 1413214 の反応式
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]

参加物

6

反応物 3

HCID 517045Sodium AcetateHCID 202940332-Bromo-4-chloroacetamidothiazoleHCID 178418361HCID 178418361、化合物

生成物 1

HCID 202940394-Chloroacetamidothiazole収率 57.9%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-fe2c8561a9974687921e79e9c14c945e
出典データセット
uspto-grants-1981_02
特許番号
US04249012

反応ノート

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