Potassium Carbonate → HCID 22509303、化合物

HRID 984876ノート

反応式

HRID 984876 の反応式
Cl[C:2]1[N:7]=[CH:6][C:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:4][N:3]=1.[C:13]([C:17]1[CH:18]=[C:19]([CH:21]=[C:22]([C:24]([CH3:27])([CH3:26])[CH3:25])[CH:23]=1)[NH2:20])([CH3:16])([CH3:15])[CH3:14].C([O-])([O-])=O.[K+].[K+]>O>[C:24]([C:22]1[CH:21]=[C:19]([NH:20][C:2]2[N:7]=[CH:6][C:5]([C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:4][N:3]=2)[CH:18]=[C:17]([C:13]([CH3:16])([CH3:15])[CH3:14])[CH:23]=1)([CH3:27])([CH3:26])[CH3:25]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 754193,5-Di-tert-butylanilineHCID 104878152-Chloro-pyrimidine-5-carboxylic acid ethyl ester

生成物 1

HCID 22509303HCID 22509303、化合物収率 90%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
110 °C

実験手順

A mixture of ethyl 2-chloropyrimidine-5-carboxylate (335 mg), 3,5-di-tert-butylaniline (370 mg), and K2CO3 (600 mg) was heated at 110° C. After the disappearance of the materials was observed with TLC, the reaction mixture was poured into water, and extracted with CH2Cl2. The organic layer was dried over Na2SO4, and the solvent was evaporated. The residue was purified by silica gel flash column chromatography (n-hexane: AcOEt=10:1) to give white crystals of ethyl 2-[N-(3,5-di-tert-butylphenyl)amino]pyrimidine-5-carboxylate (574 mg, 90%).

後処理

  1. extractionextracted with CH2Cl2
  2. dry with materialThe organic layer was dried over Na2SO4
  3. customthe solvent was evaporated
  4. customThe residue was purified by silica gel flash column chromatography (n-hexane: AcOEt=10:1)

出典と根拠

ORDレコード
ord-7e4ed6b11c3048eaa311080f6a7276d1
出典データセット
uspto-grants-2005_03
特許番号
US06869959B1

反応ノート

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