Methylamine → N-methyl-1-(3-nitrophenyl)methanesulfonamide

HRID 1891000노트

반응식

HRID 1891000 반응식
[CH3:1][NH2:2].[N+:3]([C:6]1[CH:7]=[C:8]([CH2:12][S:13](Cl)(=[O:15])=[O:14])[CH:9]=[CH:10][CH:11]=1)([O-:5])=[O:4]>C1C=CC=CC=1>[N+:3]([C:6]1[CH:7]=[C:8]([CH2:12][S:13]([NH:2][CH3:1])(=[O:15])=[O:14])[CH:9]=[CH:10][CH:11]=1)([O-:5])=[O:4]

참가 물질

4

반응물 2

HCID 6329MethylamineHCID 13196775(3-Nitrophenyl)methanesulfonyl chloride

생성물 1

HCID 13286046N-methyl-1-(3-nitrophenyl)methanesulfonamide수율 87.7%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

40% aqueous methylamine (10 mL, 0.1 mol) was added to a vigorously stirred solution of (3-Nitrophenyl)methanesulfonyl chloride (1.18 g, 5 mmol) in benzene (30 mL) and allowed to stir for 2 h at room temperature. To this end, the benzene layer was separated, and the aqueous layer extracted with CH2Cl2 (2×25 mL). The combined organic layers were washed with saturated aqueous NaHCO3 (30 mL), water (30 mL), filtered over anhydrous Na2SO4, filtered and the solvent removed under reduced pressure to give 1.01 g (87%) of (3-nitrophenyl)-N-methylmethanesulfonamide as colorless crystals.

후처리

  1. customTo this end, the benzene layer was separated
  2. extractionthe aqueous layer extracted with CH2Cl2 (2×25 mL)
  3. washThe combined organic layers were washed with saturated aqueous NaHCO3 (30 mL), water (30 mL)
  4. filtrationfiltered over anhydrous Na2SO4
  5. filtrationfiltered
  6. customthe solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-a2ef2018ab324f2482fe20ffa3f88998
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08507498B2

반응 노트

불러오는 중…