Dimethylamine → N,N-dimethyl-4-nitrobenzenesulfonamide

HRID 1484831

反応式

HRID 1484831 の反応式
[CH3:1][NH:2][CH3:3].CCN(C(C)C)C(C)C.[N+:13]([C:16]1[CH:21]=[CH:20][C:19]([S:22](Cl)(=[O:24])=[O:23])=[CH:18][CH:17]=1)([O-:15])=[O:14]>C(Cl)Cl>[CH3:1][N:2]([CH3:3])[S:22]([C:19]1[CH:18]=[CH:17][C:16]([N+:13]([O-:15])=[O:14])=[CH:21][CH:20]=1)(=[O:23])=[O:24]

参加物

5

反応物 3

HCID 674DimethylamineHCID 74044-Nitrobenzenesulfonyl chlorideHCID 81531Diisopropylethylamine

生成物 1

HCID 2747580N,N-dimethyl-4-nitrobenzenesulfonamide収率 91%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To the solution of dimethylamine (284 mg, 6.3 mmol, 1.5 equiv.) and DIPEA (1 mL) in DCM (15 mL) was added dropwise a solution of 4-nitrobenzene-1-sulfonyl chloride (800 mg, 4.2 mmol, 1.0 equiv.) in DCM (5 mL). The reaction mixture was stirred at room temperature for 2 h. Then, the reaction mixture was washed with water and brine. The organic layers was dried (Na2SO4) and concentrated to get the residue, which was washed with isopropyl ether to afford compound N,N-dimethyl-4-nitrobenzenesulfonamide (879 mg, 91%).

後処理

  1. washThen, the reaction mixture was washed with water and brine
  2. dry with materialThe organic layers was dried (Na2SO4)
  3. concentrationconcentrated
  4. customto get the residue, which
  5. washwas washed with isopropyl ether

出典と根拠

ORDレコード
ord-bb57abf62e43442b94674328fd6e7599
出典データセット
uspto-grants-2016_08
特許番号
US09422271B2

関連ノート

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