Water → HCID 67026756、化合物

HRID 12089ノート

反応式

HRID 12089 の反応式
Cl[C:2]1[N:7]=[C:6]([N:8]([CH2:10][CH3:11])[CH3:9])[C:5]([Cl:12])=[CH:4][N:3]=1.[N+:13]([C:16]1[C:21]([CH3:22])=[CH:20][C:19]([OH:23])=[C:18]([CH3:24])[CH:17]=1)([O-:15])=[O:14].C(=O)([O-])[O-].[K+].[K+].O>CN(C=O)C>[Cl:12][C:5]1[C:6]([N:8]([CH2:10][CH3:11])[CH3:9])=[N:7][C:2]([O:23][C:19]2[CH:20]=[C:21]([CH3:22])[C:16]([N+:13]([O-:15])=[O:14])=[CH:17][C:18]=2[CH3:24])=[N:3][CH:4]=1

参加物

6

反応物 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 2821102,5-Dimethyl-4-nitrophenolHCID 79631958HCID 79631958、化合物

生成物 1

HCID 67026756HCID 67026756、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A solution of 16.8 g (40 mmol) 2,5-dichloro-N-ethyl-N-methylpyrimidin-4-amine, 7.35 g 4-nitro-2,5-dimethylphenol (44 mmol) and 8.29 g potassium carbonate (60 mmol) in 70 ml DMF were stirred for 20 hrs at 100° C. After adding the mixture to 150 ml water the resulting suspension was extracted twice with 50 ml dichloromethane. The combined organic layers were washed with aqueous solution of sodium hydroxide. The organic layer was dried over magnesium sulfate, concentrated in vacuo and column chromatography (dichloromethane) yielded 8.3 g (47%) with a purity of 76%; log P (pH=2.3)=4.07.

後処理

  1. extractionwas extracted twice with 50 ml dichloromethane
  2. washThe combined organic layers were washed with aqueous solution of sodium hydroxide
  3. dry with materialThe organic layer was dried over magnesium sulfate
  4. concentrationconcentrated in vacuo and column chromatography (dichloromethane)
  5. customyielded 8.3 g (47%) with a purity of 76%

出典と根拠

ORDレコード
ord-aa3196a16d9a4431bf69a02926667947
出典データセット
uspto-grants-2010_06
特許番号
US07727986B2

反応ノート

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