Methanesulfonyl chloride → HCID 68511606, 화합물

HRID 1716295노트

반응식

HRID 1716295 반응식
[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

참가 물질

5

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 68512931HCID 68512931, 화합물

생성물 1

HCID 68511606HCID 68511606, 화합물

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 21875418Pyridine methylene chloride용매

실험 절차

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)+.

후처리

  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)

출처 및 근거

ORD 기록
ord-6622d5547d9c4579bbe6e7789cc39e28
출처 데이터셋
uspto-grants-2010_09
특허 번호
US07803793B2

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