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

HRID 1941915ノート

反応式

HRID 1941915 の反応式
[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]

参加物

4

反応物 2

HCID 6329MethylamineHCID 13196775(3-Nitrophenyl)methanesulfonyl chloride

生成物 1

HCID 13286046N-methyl-1-(3-nitrophenyl)methanesulfonamide収率 90%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

40% aqueous methylamine (10 mL, 0.1 mol) was added to a vigorously stirred solution of (3-nitrophenyl)methanesulfonyl chloride (2.36 g, 10 mmol) in benzene (30 mL) and allowed to stir for 2 h at room temperature. 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 2.07 g (90%) of (3-nitrophenyl)-N-methylmethanesulfonamide as crystals.

後処理

  1. customThe 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

出典と根拠

ORDレコード
ord-c854b0b7c3654929b69bc4429e777ffa
出典データセット
uspto-grants-2013_03
特許番号
US08389521B2

反応ノート

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