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

HRID 81354

반응식

HRID 81354 반응식
[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

참가 물질

5

반응물 3

HCID 10796Cesium carbonateHCID 2372592,4,5-TrichloropyrimidineHCID 585225447-hydroxy-2-methyl-2,3-dihydro-1H-isoindol-1-one

생성물 1

HCID 585225547-(2,5-Dichloro-pyrimidin-4-yloxy)-2-methyl-2,3-dihydro-isoindol-1-one

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-434867972c824e36b147a39657cc7d76
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846689B2

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