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

HRID 1890985ノート

反応式

HRID 1890985 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. 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 2.07 g (90%) of (3-nitrophenyl)-N-methylmethanesulfonamide as crystals.

後処理

  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

出典と根拠

ORDレコード
ord-754a9fb05f804bd99e1a4df8258c53bd
出典データセット
uspto-grants-2013_08
特許番号
US08507498B2

反応ノート

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