Methanesulfonyl chloride → HCID 68511606、化合物

HRID 1716295ノート

反応式

HRID 1716295 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH2:10][NH:11][C:12]2[CH:17]=[CH:16][C:15]([O:18][C:19]3[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][CH:20]=3)=[CH:14][CH:13]=2)[C:5]([O:8][CH3:9])=[N:6][CH:7]=1.[CH3:26][S:27](Cl)(=[O:29])=[O:28]>C(Cl)Cl.N1C=CC=CC=1.C(Cl)Cl>[Br:1][C:2]1[CH:3]=[C:4]([CH2:10][N:11]([C:12]2[CH:13]=[CH:14][C:15]([O:18][C:19]3[CH:24]=[CH:23][C:22]([CH3:25])=[CH:21][CH:20]=3)=[CH:16][CH:17]=2)[S:27]([CH3:26])(=[O:29])=[O:28])[C:5]([O:8][CH3:9])=[N:6][CH:7]=1

参加物

5

反応物 2

HCID 31297Methanesulfonyl chlorideHCID 68512931HCID 68512931、化合物

生成物 1

HCID 68511606HCID 68511606、化合物

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 21875418Pyridine methylene chloride溶媒

実験手順

To a solution of (5-bromo-2-methoxy-pyridin-3-ylmethyl)-(4-p-tolyloxy-phenyl)-amine (0.73 g, 1.82 mmol) from Step A in CH2Cl2/pyridine (6 mL/3 mL) was dropwise added methylsulfonyl chloride (0.17 mL, 2.2 mmol) at 0° C. The resulting mixture was warmed to room temperature and stirred overnight. The reaction was then diluted with CH2Cl2 and washed with aqueous HCl (3N) to remove pyridine. The organic layer was then brought to the usual work-up. The crude product was purified by chromatography (silica gel, 30% EtOAc/hexanes). MS (EI) 477, 479 (M+H)+.

後処理

  1. customat 0° C
  2. washwashed with aqueous HCl (3N)
  3. customto remove pyridine
  4. customThe crude product was purified by chromatography (silica gel, 30% EtOAc/hexanes)

出典と根拠

ORDレコード
ord-6622d5547d9c4579bbe6e7789cc39e28
出典データセット
uspto-grants-2010_09
特許番号
US07803793B2

反応ノート

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