Methylamine → N-Methyl-4-nitrobenzenesulfonamide

HRID 57230노트

반응식

HRID 57230 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10](Cl)(=[O:12])=[O:11])=[CH:6][CH:5]=1)([O-:3])=[O:2].[CH2:14]([N:16](CC)CC)C.CN>C1COCC1.[Cl-].[Na+].O>[CH3:14][NH:16][S:10]([C:7]1[CH:8]=[CH:9][C:4]([N+:1]([O-:3])=[O:2])=[CH:5][CH:6]=1)(=[O:12])=[O:11]

참가 물질

6

반응물 3

HCID 6329MethylamineHCID 74044-Nitrobenzenesulfonyl chlorideHCID 8471Triethylamine

생성물 1

HCID 232993N-Methyl-4-nitrobenzenesulfonamide

시약·촉매·용매 2

HCID 8028Tetrahydrofuran용매2회HCID 57417360Sodium chloride; water용매

실험 절차

To an ice cold solution of 4-nitrobenzenesulfonyl chloride (2.7 g, 12 mmol) and triethylamine (27 mmol) in 60 mL of dry THF was added methylamine (8 mL of a 2 M solution in THF, 16 mmol). The mixture was stirred at room temperature overnight. Brine was added and the reaction solution was extracted with ethyl acetate. The combined organic extracts were dried over sodium sulfate, filtered, and evaporated to yield 4-nitrobenzenesulfonic acid methylamide as an oil. The crude material was used in the subsequent reaction without further purification.

후처리

  1. extractionthe reaction solution was extracted with ethyl acetate
  2. dry with materialThe combined organic extracts were dried over sodium sulfate
  3. filtrationfiltered
  4. customevaporated

출처 및 근거

ORD 기록
ord-a67356e0507b4344a8b72abc7c120994
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09434720B2

반응 노트

불러오는 중…