Sodium Acetate → 4-Acetamidothiazole

HRID 1413206ノート

反応式

HRID 1413206 の反応式
[C:1]([NH:4][C:5]1[N:6]=[C:7](Br)[S:8][CH:9]=1)(=[O:3])[CH3:2].C([O-])(=O)C.[Na+].[H][H]>CO.[Pd]>[C:1]([NH:4][C:5]1[N:6]=[CH:7][S:8][CH:9]=1)(=[O:3])[CH3:2]

参加物

6

反応物 3

HCID 517045Sodium AcetateHCID 202940434-Acetamido-2-bromo-thiazoleHCID 178418361HCID 178418361、化合物

生成物 1

HCID 202940374-Acetamidothiazole収率 84.8%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 887Methanol溶媒

実験手順

A solution of 4-acetamido-2-bromo-thiazole (22 g., 0.2 m) and sodium acetate (8.2 g, 0.1 m) in methanol (600 ml) was hydrogenated at room temperature and 1 atm. pressure oven 10% palladium on carbon (5 g) until the theoretical uptake of hydrogen had occurred (about 3 hours). The catalyst was removed by filtration and the filtrate evaporated to dryness under reduced pressure. The residue was extracted with carbon tetrachloride (200 ml) in a Soxlet apparatus. The extract was cooled and the crystals removed by filtration to yield 4-acetamidothiazole (12 g, 78%). m.p. 176° C. Found: C, 41.8; H, 4.3; N, 19.3. C5H6N2OS requires: C, 42.2; H, 4.3; N, 19.7%.

後処理

  1. customwas hydrogenated at room temperature
  2. custom(about 3 hours)
  3. customThe catalyst was removed by filtration
  4. customthe filtrate evaporated to dryness under reduced pressure
  5. extractionThe residue was extracted with carbon tetrachloride (200 ml) in a Soxlet apparatus
  6. temperatureThe extract was cooled
  7. customthe crystals removed by filtration

出典と根拠

ORDレコード
ord-ea92f29ea8794b19b3f1042fc68f7cfc
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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