Methyl iodide → 4-[4-(Methylsulfonyl)phenyl]-N-methyl-N-tetrahydro-2H-pyran-4-yl-6-(trifluoromethyl)pyrimidin-2-amine

HRID 6697

반응식

HRID 6697 반응식
[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[C:15]([C:17]([F:20])([F:19])[F:18])[N:14]=[C:13]([NH:21][CH:22]3[CH2:27][CH2:26][O:25][CH2:24][CH2:23]3)[N:12]=2)=[CH:7][CH:6]=1)(=[O:4])=[O:3].[H-].[Na+].I[CH3:31]>CN(C)C=O>[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[C:15]([C:17]([F:20])([F:19])[F:18])[N:14]=[C:13]([N:21]([CH3:31])[CH:22]3[CH2:27][CH2:26][O:25][CH2:24][CH2:23]3)[N:12]=2)=[CH:7][CH:6]=1)(=[O:3])=[O:4]

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 98223574-(4-(methylsulfonyl)phenyl)-N-(tetrahydro-2H-pyran-4-yl)-6-(trifluoromethyl)pyrimidin-2-amine

생성물 1

HCID 101365794-[4-(Methylsulfonyl)phenyl]-N-methyl-N-tetrahydro-2H-pyran-4-yl-6-(trifluoromethyl)pyrimidin-2-amine

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 4-[4-(methylsulfonyl)phenyl]-N-tetrahydro-2H-pyran-4-yl-6-(trifluoromethyl)pyrimidin-2-amine (0.05 g) in dry dimethylformamide (2 ml) was treated with sodium hydride (0.007 g, 60% in mineral oil) and the mixture stirred at ambient temperature for 30 minutes. Iodomethane (0.01 ml) was added and the mixture stirred overnight. The reaction mixture was concentrated in vacuo and the residue partitioned between dichloromethane (20 ml) and water (20 ml). The organic layer was purified by passing through a silica bond elute column and eluting with dichloromethane. Concentration of the eluent gave the title compound as a yellow solid (0.031 g).

후처리

  1. stirringthe mixture stirred overnight
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. customthe residue partitioned between dichloromethane (20 ml) and water (20 ml)
  4. customThe organic layer was purified
  5. washelute column
  6. washeluting with dichloromethane

출처 및 근거

ORD 기록
ord-7489cadc00124f82a4089f651da7299f
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07084148B2

연결된 노트

불러오는 중…