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

HRID 1167240노트

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HRID 1167240 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

HCID 2921148N,N,2-trimethyl-5-nitro-Benzenesulfonamide수율 85%

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

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온도
0 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-ccf2205cada4479ea9390f52bd9b2e83
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06617357B2

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