Allyl Alcohol → HCID 20482369、化合物

HRID 648183ノート

反応式

HRID 648183 の反応式
[H-].[Na+].[CH2:3]([OH:6])[CH:4]=[CH2:5].[H][H].Br[C:10]1[S:11][C:12]([C:15](=[O:19])[N:16]([CH3:18])[CH3:17])=[CH:13][N:14]=1>CN(C)C=O.O>[CH2:3]([O:6][C:10]1[S:11][C:12]([C:15](=[O:19])[N:16]([CH3:18])[CH3:17])=[CH:13][N:14]=1)[CH:4]=[CH2:5]

参加物

7

反応物 4

HCID 7858Allyl AlcoholHCID 24758Sodium hydrideHCID 204823682-bromo-N,N-dimethyl-1,3-thiazole-5-carboxamideHCID 178418361HCID 178418361、化合物

生成物 1

HCID 20482369HCID 20482369、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a stirred suspension of 0.5 g (10 mmol) of sodium hydride in 5 ml of dry N,N-di-methylformamide under N2, there can be added 0.6 g (10 mmol) of sieve-dried allyl alcohol. After hydrogen evolution ceases, the stirred solution can be treated with 2-bromo-5-(N,N-dimethylcarbamoyl)thiazole (2.35 g, 10.0 mmole). The mixture can then be stirred at 40° under N2 for 18 hours, diluted with four volumes of water and extracted with ether. The ether extracts can be washed with water, dried (Na2SO4), filtered and concentrated in vacuo to give an oil which can then be distilled to give pure title compound.

後処理

  1. extractionextracted with ether
  2. washThe ether extracts can be washed with water
  3. dry with materialdried (Na2SO4)
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customto give an oil which
  7. distillationcan then be distilled

出典と根拠

ORDレコード
ord-fe7237d345e04ac1b1577aef2ef9156c
出典データセット
uspto-grants-1983_10
特許番号
US04411899

反応ノート

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