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Thioacetamide → Ethyl 2-(2-methylthiazol-5-yl)acetate

HRID 972834
ノート
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反応式

HRID 972834 の反応式
Br[CH:2]([CH:9]=O)[CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5].[C:11]([NH2:14])(=[S:13])[CH3:12]>ClC(Cl)C>[CH3:12][C:11]1[S:13][C:2]([CH2:3][C:4]([O:6][CH2:7][CH3:8])=[O:5])=[CH:9][N:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 2723949ThioacetamideHCID 15576269Ethyl 3-bromo-4-oxobutanoate

生成物 1

HCID 20388951Ethyl 2-(2-methylthiazol-5-yl)acetate収率 32.6%

試薬・触媒・溶媒 1

HCID 63651,1-Dichloroethane溶媒2 回

実験手順

A mixture of 28.7 g of ethyl 3-bromo-4-oxo-butyrate, 300 ml of dichloroethane and 11.2 g of thioacetamide was refluxed for 10 hours with stirring while replacing the dichloroethane that distilled to keep the volume constant and then the mixture was cooled to room temperature. The mixture was evaporated to dryness and the residue was dissolved in ethyl acetate. The solution was extracted with 2N hydrochloric acid and the pH of the aqueous extracts was made alkaline by addition of ammonium hydroxide. The mixture was extracted with ethyl acetate and the organic extract was washed with water, dried and evaporated to dryness to obtain 8.3 g of ethyl 2-methyl-5-thiazole acetate. The IR spectrum in CHCl3 showed ester C=O at 1737cm-1 and C=C and C=N at 1535cm-1.

後処理

  1. temperaturewas refluxed for 10 hours
  2. distillationthat distilled
  3. customThe mixture was evaporated to dryness
  4. dissolutionthe residue was dissolved in ethyl acetate
  5. extractionThe solution was extracted with 2N hydrochloric acid
  6. additionby addition of ammonium hydroxide
  7. extractionThe mixture was extracted with ethyl acetate
  8. extractionthe organic extract
  9. washwas washed with water
  10. customdried
  11. customevaporated to dryness

出典と根拠

ORDレコード
ord-2019cab32ea346b89823cb91605b7429
出典データセット
uspto-grants-1977_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04053618

反応ノート

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