Sodium hydride → HCID 67281141, 화합물

HRID 1694718노트

반응식

HRID 1694718 반응식
[H-].[Na+].[CH2:3]([NH:10][C:11]1[N:16]=[CH:15][C:14]([Br:17])=[CH:13][N:12]=1)[C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][CH:5]=1.[CH3:18][S:19](Cl)(=[O:21])=[O:20]>CN(C=O)C>[Br:17][C:14]1[CH:15]=[N:16][C:11]([N:10]([CH2:3][C:4]2[CH:5]=[CH:6][CH:7]=[CH:8][CH:9]=2)[S:19]([CH3:18])(=[O:21])=[O:20])=[N:12][CH:13]=1

참가 물질

5

반응물 3

HCID 24758Sodium hydrideHCID 31297Methanesulfonyl chlorideHCID 51391422-BENZYLAMINO-5-BROMOPYRIMIDINE

생성물 1

HCID 67281141HCID 67281141, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

Sodium hydride (0.1 g, 60% disp. in oil) was added to a stirred solution of benzyl-(5-bromo-pyrimidin-2-yl)-amine (0.55 g) in DMF (8 ml) at 0° C. After 30 min methanesulphonyl chloride (0.286 g) was added and the mixture stirred at RT for 2 h then partitioned between ethyl acetate and water. The organics were separated washed with water, dried and evaporated under reduced pressure. The residue was purified by chromatography on silica eluting with dichloromethane. Yield 0.41 g

후처리

  1. customthen partitioned between ethyl acetate and water
  2. customThe organics were separated
  3. washwashed with water
  4. customdried
  5. customevaporated under reduced pressure
  6. customThe residue was purified by chromatography on silica eluting with dichloromethane

출처 및 근거

ORD 기록
ord-8ac5083582b54a5881861183c061f556
출처 데이터셋
uspto-grants-2012_04
특허 번호
US08158820B2

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