Methylamine → 4-amino-N-methylbenzene-1-sulfonamide

HRID 23921ノート

反応式

HRID 23921 の反応式
CN.[CH2:3]([N:5](CC)CC)C.[S:10](F)(=[O:19])([C:12]1[CH:17]=[CH:16][C:15]([NH2:18])=[CH:14][CH:13]=1)=[O:11]>C(O)C>[CH3:3][NH:5][S:10]([C:12]1[CH:17]=[CH:16][C:15]([NH2:18])=[CH:14][CH:13]=1)(=[O:19])=[O:11]

参加物

5

反応物 3

HCID 6329MethylamineHCID 8471TriethylamineHCID 668234-Aminobenzenesulfonyl fluoride

生成物 1

HCID 743684-amino-N-methylbenzene-1-sulfonamide収率 78.1%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
80 °C

実験手順

Methylamine (3 ml of a 33% solution in ethanol) and then triethylamine (0.159 ml, 1.1 mmol) was added to sulphanilyl fluoride (200 mg, 1.1 mmol), and the mixture heated at 80° C. for 6 hours then at ambient temperature for 18 hours. The volatiles were removed by evaporation and the residue azeotroped with toluene to give the title compound (160 mg, 76%). NMR: 2.30 (s, 3H), 5.85 (s, 2H), 6.60 (d, 2H), 7.39 (d, 2H); m/z: 187 [MH]+.

後処理

  1. customThe volatiles were removed by evaporation
  2. customthe residue azeotroped with toluene

出典と根拠

ORDレコード
ord-6672536baecc4bce82f56c30b796dbe9
出典データセット
uspto-grants-2005_02
特許番号
US06855719B1

反応ノート

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