Ammonium Hydroxide → 6-Chloro-2-methylpyrimidin-4-amine

HRID 359684

반응식

HRID 359684 반응식
[Cl:1][C:2]1[CH:7]=[C:6](Cl)[N:5]=[C:4]([CH3:9])[N:3]=1.[OH-].[NH4+:11]>COCCOC.O>[Cl:1][C:2]1[N:3]=[C:4]([CH3:9])[N:5]=[C:6]([NH2:11])[CH:7]=1

참가 물질

5

반응물 2

HCID 14923Ammonium HydroxideHCID 2349974,6-Dichloro-2-methylpyrimidine

생성물 1

HCID 2867546-Chloro-2-methylpyrimidin-4-amine수율 60%

시약·촉매·용매 2

HCID 962Water용매HCID 80711,2-Dimethoxyethane용매

반응 조건

온도
23 °C

실험 절차

A stirred suspension of 4,6-dichloro-2-methylpyrimidine (39.5 g, 244 mmol) in 1,2-dimethoxyethane (50 mL) in a sealable pressure reaction vessel was treated with concentrated aqueous ammonium hydroxide (40 mL). The mixture was vigorously stirred at 23° C. for 14 days in the sealed vessel. The mixture was then diluted with water and filtered. The isolated white solids were rinsed with water and dried in vacuo to afford 6-chloro-2-methyl-4-aminopyrimidine (20.94 g, 146 mmol, 60% yield): mp 191°-192° C.; Rf 0.49 (EtOAc); 1H NMR (DMSO-D6, 200 MHz)δ7.09 (br s, 2H, NH), 6.24 (s, 1H), 2.26 (s, 3H).

후처리

  1. customin a sealable pressure reaction vessel
  2. filtrationfiltered
  3. washThe isolated white solids were rinsed with water
  4. customdried in vacuo

출처 및 근거

ORD 기록
ord-282dad6dae8d4dde8905dd9855fe88cb
출처 데이터셋
uspto-grants-1991_03
특허 번호
US05002949

연결된 노트

불러오는 중…