Potassium Carbonate → HCID 86622894、化合物

HRID 643499ノート

反応式

HRID 643499 の反応式
[C:1]([O:5][C:6](=[O:22])[NH:7][CH2:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([OH:21])[CH:16]=2)=[CH:11][CH:10]=1)([CH3:4])([CH3:3])[CH3:2].[Cl:23][C:24]1[N:29]=[C:28](Cl)[CH:27]=[CH:26][N:25]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C=O)C>[C:1]([O:5][C:6](=[O:22])[NH:7][CH2:8][C:9]1[CH:14]=[CH:13][C:12]([C:15]2[CH:20]=[CH:19][CH:18]=[C:17]([O:21][C:26]3[CH:27]=[CH:28][N:29]=[C:24]([Cl:23])[N:25]=3)[CH:16]=2)=[CH:11][CH:10]=1)([CH3:4])([CH3:2])[CH3:3]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 775312,4-DichloropyrimidineHCID 67456175HCID 67456175、化合物

生成物 1

HCID 86622894HCID 86622894、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of (3′-hydroxy-biphenyl-4-ylmethyl)-carbamic acid tert-butyl ester (435 mg), 2,4-dichloropyrimidine (221 mg) and potassium carbonate (295 mg) in DMF (10 ml) is stirred at rt for 20 h. This mixture is quenched with brine and extracted twice with EtOAc. The combined organic phases are dried over sodium sulfate, the solvent is evaporated and the resulting crude product is purified on silica (90 g) with cyclohexane/EtOAc 80/20 to afford pure [3′-(2-chloro-pyrimidin-4-yloxy)-biphenyl-4-ylmethyl]-carbamic acid tert-butyl ester.

後処理

  1. customThis mixture is quenched with brine
  2. extractionextracted twice with EtOAc
  3. dry with materialThe combined organic phases are dried over sodium sulfate
  4. customthe solvent is evaporated
  5. customthe resulting crude product is purified on silica (90 g) with cyclohexane/EtOAc 80/20

出典と根拠

ORDレコード
ord-502855607dd2439fa85b4c0c40e07be4
出典データセット
uspto-grants-2010_04
特許番号
US07700605B2

反応ノート

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