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Methanesulfonyl chloride → HCID 86679430, 화합물

HRID 1776477
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HRID 1776477 반응식
[CH:1]1([CH2:4][O:5][C:6]2[CH:12]=[CH:11][CH:10]=[CH:9][C:7]=2[NH2:8])[CH2:3][CH2:2]1.[CH3:13][S:14](Cl)(=[O:16])=[O:15]>N1C=CC=CC=1>[CH:1]1([CH2:4][O:5][C:6]2[CH:12]=[CH:11][CH:10]=[CH:9][C:7]=2[NH:8][S:14]([CH3:13])(=[O:16])=[O:15])[CH2:2][CH2:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 31297Methanesulfonyl chlorideHCID 196269232-(Cyclopropylmethoxy)aniline

생성물 1

HCID 86679430HCID 86679430, 화합물수율 96%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A solution of 2-(cyclopropylmethoxy)aniline (1.03 g, 6.31 mmol) in pyridine (20 ml) was cooled to 0° C., and methanesulfonyl chloride (0.541 ml, 6.94 mmol) was added. The mixture was warmed to RT and stirred for 2 hours. The solvent was removed, and the crude was portioned between EtOAc and HCl 1N. The organic phase was washed with brine and dried over Na2SO4. The solvent was removed and the crude was purified by filtration on silica gel cartridge (petroleum ether:EtOAc=80:20) affording N-(2-(cyclopropylmethoxy)phenyl)methanesulfonamide (1.456 g, 6.03 mmol, 96% yield, MS/ESI+ 263.9 [MNa]+).

후처리

  1. customThe solvent was removed
  2. washThe organic phase was washed with brine
  3. dry with materialdried over Na2SO4
  4. customThe solvent was removed
  5. filtrationthe crude was purified by filtration on silica gel cartridge (petroleum ether:EtOAc=80:20)

출처 및 근거

ORD 기록
ord-77fa96ab6cbb42be897c6d7004b76095
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09265768B2

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