Hydrochloric Acid → 2-Pyridin-2-yl-thiazol-5-ylamine

HRID 1260324ノート

反応式

HRID 1260324 の反応式
C(OC(=O)[NH:7][C:8]1[S:12][C:11]([C:13]2[CH:18]=[CH:17][CH:16]=[CH:15][N:14]=2)=[N:10][CH:9]=1)(C)(C)C.Cl>O1CCOCC1>[N:14]1[CH:15]=[CH:16][CH:17]=[CH:18][C:13]=1[C:11]1[S:12][C:8]([NH2:7])=[CH:9][N:10]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 67299899(2-Pyridin-2-yl-thiazol-5-yl)-carbamic acid tert-butyl ester

生成物 1

HCID 457887092-Pyridin-2-yl-thiazol-5-ylamine収率 61.1%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

A solution of (2-pyridin-2-yl-thiazol-5-yl)-carbamic acid tert-butyl ester (200 mg, 0.72 mmol) in dioxane (3 ml) was treated with 4M HCl in dioxane (3 ml) and the resulting suspension was stirred at ambient temperature overnight. The reaction mixture was filtrated and the precipitate was dissolved in sodium hydroxide (20 ml, 0.5M aqueous solution) and extracted with dichloromethane. The combined organic phases were dried and the solvent was evaporated to yield the product as orange solid (78 mg, 60%) which was used without any further purification. MS: M=178.1 (M+H)+

後処理

  1. filtrationThe reaction mixture was filtrated
  2. dissolutionthe precipitate was dissolved in sodium hydroxide (20 ml, 0.5M aqueous solution)
  3. extractionextracted with dichloromethane
  4. customThe combined organic phases were dried
  5. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-541a556610bf41adbb89e0bba3fa2393
出典データセット
uspto-grants-2013_06
特許番号
US08470820B2

反応ノート

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