Sodium hydride → HCID 67281141、化合物

HRID 1694718ノート

反応式

HRID 1694718 の反応式
[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

参加物

5

反応物 3

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

生成物 1

HCID 67281141HCID 67281141、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

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

後処理

  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

出典と根拠

ORDレコード
ord-8ac5083582b54a5881861183c061f556
出典データセット
uspto-grants-2012_04
特許番号
US08158820B2

反応ノート

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