Methanesulfonyl chloride → HCID 20306015, 화합물

HRID 1732338노트

반응식

HRID 1732338 반응식
[CH3:1][S:2](Cl)(=[O:4])=[O:3].[CH3:6][O:7][C:8]1[CH:17]=[CH:16][CH:15]=[C:14]([O:18][CH3:19])[C:9]=1[O:10][CH2:11][CH2:12][OH:13]>N1C=CC=CC=1>[S:2]([O:13][CH2:12][CH2:11][O:10][C:9]1[C:8]([O:7][CH3:6])=[CH:17][CH:16]=[CH:15][C:14]=1[O:18][CH3:19])(=[O:4])(=[O:3])[CH3:1]

참가 물질

4

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 142576012-(2,6-Dimethoxyphenoxy)ethan-1-ol

생성물 1

HCID 20306015HCID 20306015, 화합물수율 40.5%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

Methanesulphonyl chloride (23 g.) was added dropwise to a stirred solution of 2-[2,6-dimethoxyphenoxy]ethanol (20 g.) (J. Med. Chem. 1969, 12, 326) in pyridine (50 ml.). The solution was left at room temperature for 60 hours, then the solvent evaporated under reduced pressure. The residue was taken up in chloroform, washed with water (3×100 ml.) and sodium bicarbonate solution (5%, 3×100 ml.), dried and the solvent evaporated. The residue was triturated with n-hexane and the solid collected to give 2-[2,6-dimethoxyphenoxy]-ethyl mesylate (11.3 g.) characterized spectroscopically.

후처리

  1. customthe solvent evaporated under reduced pressure
  2. washwashed with water (3×100 ml.) and sodium bicarbonate solution (5%, 3×100 ml.)
  3. customdried
  4. customthe solvent evaporated
  5. customThe residue was triturated with n-hexane
  6. customthe solid collected

출처 및 근거

ORD 기록
ord-0376ac52247c46a4a070b6e6b4f1e4ab
출처 데이터셋
uspto-grants-1980_12
특허 번호
US04237138

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