Cesium carbonate → 7-(2,5-Dichloro-pyrimidin-4-yloxy)-2-methyl-2,3-dihydro-isoindol-1-one

HRID 81354

反応式

HRID 81354 の反応式
[Cl:1][C:2]1[N:7]=[C:6](Cl)[C:5]([Cl:9])=[CH:4][N:3]=1.[OH:10][C:11]1[CH:12]=[CH:13][CH:14]=[C:15]2[C:19]=1[C:18](=[O:20])[N:17]([CH3:21])[CH2:16]2.C(=O)([O-])[O-].[Cs+].[Cs+]>C(Cl)Cl>[Cl:1][C:2]1[N:7]=[C:6]([O:10][C:11]2[CH:12]=[CH:13][CH:14]=[C:15]3[C:19]=2[C:18](=[O:20])[N:17]([CH3:21])[CH2:16]3)[C:5]([Cl:9])=[CH:4][N:3]=1

参加物

5

反応条件

温度
0 °C

実験手順

2,4,5-trichloropyrimidine (0.20 g) and 7-hydroxy-2-methyl-2,3-dihydro-isoindol-1-one are dissolved in DCM (10 mL), cooled to 0° C. and combined with caesium carbonate (0.75 g). The cooling bath is removed and the mixture is stirred for 16 h. For working up the mixture is combined with 10% NaCl solution (100 mL) and extracted three times with 75 mL ethyl acetate. The combined organic phases are dried on magnesium sulphate, filtered off from the desiccant and the solvent is eliminated in vacuo.

後処理

  1. customThe cooling bath is removed
  2. extractionextracted three times with 75 mL ethyl acetate
  3. customThe combined organic phases are dried on magnesium sulphate
  4. filtrationfiltered off from the desiccant and the solvent

出典と根拠

ORDレコード
ord-434867972c824e36b147a39657cc7d76
出典データセット
uspto-grants-2014_09
特許番号
US08846689B2

関連ノート

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