Dimethylformamide → 2-Amino-4-methyl-6-(1,1,2-trifluoro-2-chloro-ethoxy)-pyrimidine

HRID 463960ノート

反応式

HRID 463960 の反応式
[NH2:1][C:2]1[N:7]=[C:6]([OH:8])[CH:5]=[C:4]([CH3:9])[N:3]=1.[Cl:10][C:11]([F:15])=[C:12]([F:14])[F:13].[OH-].[K+].CN(C)C=O>O.C(Cl)Cl>[NH2:1][C:2]1[N:3]=[C:4]([CH3:9])[CH:5]=[C:6]([O:8][C:12]([F:14])([F:13])[CH:11]([F:15])[Cl:10])[N:7]=1

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 6594ChlorotrifluoroethyleneHCID 14797Potassium HydroxideHCID 178429408HCID 178429408、化合物

生成物 1

HCID 201856922-Amino-4-methyl-6-(1,1,2-trifluoro-2-chloro-ethoxy)-pyrimidine収率 18%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

25 g of 2-amino-4-hydroxy-6-methyl-pyrimidine, 25.6 g of chlorotrifluoroethylene, 13.8 g of potassium hydroxide and 200 ml of dimethylformamide are stirred together at 60° in an autoclave for 8 hours. The mixture is diluted with water and extracted with ethyl acetate and the extract is evaporated to give a dark oil. A little methylene chloride is added and the crystalline precipitate formed is separated off to give 8.7 g of 2-amino-4-methyl-6-(1,1,2-trifluoro-2-chloro-ethoxy)-pyrimidine of melting point 73°-74° C.

後処理

  1. extractionextracted with ethyl acetate
  2. customthe extract is evaporated
  3. customto give a dark oil
  4. customthe crystalline precipitate formed
  5. customis separated off

出典と根拠

ORDレコード
ord-446a4486b0be4e8bae439d154159e210
出典データセット
uspto-grants-1985_10
特許番号
US04545811

反応ノート

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