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Dimethylformamide → 5-(2,4-Difluorophenylaminomethyl)pyrimidine

HRID 2351976
ノート
印刷プレビュー

反応式

HRID 2351976 の反応式
Cl[CH2:2][C:3]1[CH:4]=[N:5][CH:6]=[N:7][CH:8]=1.CN(C)C=O.[F:14][C:15]1[CH:21]=[C:20]([F:22])[CH:19]=[CH:18][C:16]=1[NH2:17].C(=O)(O)[O-].[Na+]>O.ClCCl>[F:14][C:15]1[CH:21]=[C:20]([F:22])[CH:19]=[CH:18][C:16]=1[NH:17][CH2:2][C:3]1[CH:4]=[N:5][CH:6]=[N:7][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 97092,4-DifluoroanilineHCID 516892Sodium BicarbonateHCID 147202965-(Chloromethyl)pyrimidine

生成物 1

HCID 147202975-(2,4-Difluorophenylaminomethyl)pyrimidine

試薬・触媒・溶媒 2

HCID 962Water溶媒
HCID 6344
Dichloromethane
溶媒

実験手順

A 26.7 g. portion of 5-chloromethylpyrimidine was dissolved in 25 ml. of dimethylformamide, and 9.4 g. of 2,4-difluoroaniline was added, followed by 6.1 g. of sodium bicarbonate. The mixture was stirred for several days with gentle heating. It was then diluted with water and extracted with ethyl acetate. The organic layer was washed with water, dried over magnesium sulfate, and evaporated under vacuum to obtain 13.75 g. of oil. The oil was dissolved in dichloromethane and purified over silica gel, eluting with dichloromethane, to obtain 4.9 g. of the desired intermediate product.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with water
  3. dry with materialdried over magnesium sulfate
  4. customevaporated under vacuum
  5. customto obtain 13.75 g
  6. custompurified over silica gel
  7. washeluting with dichloromethane
  8. customto obtain 4.9 g

出典と根拠

ORDレコード
ord-ab79d7c96d77491996b56a547c151a16
出典データセット
uspto-grants-1989_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04874775

反応ノート

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