Dimethylamine → N,N,2-trimethyl-5-nitro-Benzenesulfonamide

HRID 1167240ノート

反応式

HRID 1167240 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[S:11](Cl)(=[O:13])=[O:12].[CH3:15][NH:16][CH3:17]>CO.O>[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[S:11]([N:16]([CH3:17])[CH3:15])(=[O:13])=[O:12]

参加物

5

反応物 2

HCID 674DimethylamineHCID 8457o-Toluenesulfonyl chloride, 5-nitro-

生成物 1

HCID 2921148N,N,2-trimethyl-5-nitro-Benzenesulfonamide収率 85%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

反応条件

温度
0 °C

実験手順

To a solution of 2-methyl-5-nitrobenzenesulfonyl chloride (5.0 g, 21.2 mmol) in 100 mL of methanol at 0° C. was added dimethylamine (5.3 mL of a 40% aqueous solution). The resulting reaction mixture was stirred at 0° C. for 10 min, during which time the product crashed out as white needles. The mixture was diluted with water and filtered, washing once with water. The needles were collected and dried in vacuo to provide 2-methyl-5-nitro(N,N-dimethyl)benzenesulfonamide (4.4 g, 85%), mp 72-74° C.

後処理

  1. customThe resulting reaction mixture
  2. filtrationfiltered
  3. washwashing once with water
  4. customThe needles were collected
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-ccf2205cada4479ea9390f52bd9b2e83
出典データセット
uspto-grants-2003_09
特許番号
US06617357B2

反応ノート

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