Sodium Hydroxide → 4-Chloro-N-(4-fluorophenyl)-5,6-dimethylpyrimidin-2-amine

HRID 1069394노트

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HRID 1069394 반응식
O[C:2]1[C:7]([CH3:8])=[C:6]([CH3:9])[N:5]=[C:4]([NH:10][C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=2)[N:3]=1.P(Cl)(Cl)([Cl:20])=O.[OH-].[Na+]>CN(C)C=O>[Cl:20][C:2]1[C:7]([CH3:8])=[C:6]([CH3:9])[N:5]=[C:4]([NH:10][C:11]2[CH:16]=[CH:15][C:14]([F:17])=[CH:13][CH:12]=2)[N:3]=1

참가 물질

5

반응물 3

HCID 14798Sodium HydroxideHCID 24813Phosphorus oxychlorideHCID 178433118HCID 178433118, 화합물

생성물 1

HCID 99923764-Chloro-N-(4-fluorophenyl)-5,6-dimethylpyrimidin-2-amine수율 96.7%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
80 °C

실험 절차

40.5 g (174.1 mmole) of 2-(4-fluorophenylamino)-4-hydroxy-5,6-dimethylpyrimidine produced in Example 1 was suspended in 80 ml of N,N-dimethylformamide and the resulting suspension was heated to 80° C. 31.9 g (19.4 ml, 210.1 mmole) of phosphorus oxychloride was added thereto over one hour at constant temperature of 85° C. The reaction solution was stirred for 30 minutes and then 400 g of ice-water was added thereto with stirring. The mixture was adjusted to pH 11 by adding sodium hydroxide and then the resulting solid product was filtered. The separated solid product was washed with 150 ml of 50% aqueous methanol solution and then dried to obtain 42.3 g of the title compound.

후처리

  1. stirringwith stirring
  2. filtrationthe resulting solid product was filtered
  3. washThe separated solid product was washed with 150 ml of 50% aqueous methanol solution
  4. customdried

출처 및 근거

ORD 기록
ord-c62cba1c5c884d44a819a00b7e24e16a
출처 데이터셋
uspto-grants-2001_06
특허 번호
US06252076B1

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