Acetone → N-tert-Butyl-2-methoxy-4-nitro-benzenesulfonamide

HRID 970432노트

반응식

HRID 970432 반응식
[CH3:1][O:2][C:3]1[CH:8]=[C:7]([N+:9]([O-:11])=[O:10])[CH:6]=[CH:5][C:4]=1[S:12](Cl)(=[O:14])=[O:13].C(N(CC)CC)C.[C:23]([NH2:27])([CH3:26])([CH3:25])[CH3:24].CC(C)=O>CC(C)=O.O>[C:23]([NH:27][S:12]([C:4]1[CH:5]=[CH:6][C:7]([N+:9]([O-:11])=[O:10])=[CH:8][C:3]=1[O:2][CH3:1])(=[O:14])=[O:13])([CH3:26])([CH3:25])[CH3:24]

참가 물질

6

반응물 4

HCID 180AcetoneHCID 6385Tert-ButylamineHCID 8471TriethylamineHCID 3094582-Methoxy-4-nitrobenzenesulfonyl chloride

생성물 1

HCID 47190031N-tert-Butyl-2-methoxy-4-nitro-benzenesulfonamide

시약·촉매·용매 1

HCID 18366337Propan-2-one--water (1/1)용매

실험 절차

A solution of 5.0 g (19.9 mmol) of 2-methoxy-4-nitro-benzenesulfonyl chloride in acetone/water (60 ml/15 ml) is mixed at room temperature with 2.9 ml of triethylamine and 2.2 ml of tert.-butylamine. After 5 hours, the acetone is drawn off, and the residue is extracted from ethyl acetate. The combined organic phases are washed with dilute HCl solution and saturated NaCl solution and then filtered through a Whatman filter and concentrated by evaporation. The crude product that is obtained is recrystallized from ethyl acetate. 4.2 g (14.6 mmol, corresponding to 73% of theory) of the product is obtained.

후처리

  1. extractionthe residue is extracted from ethyl acetate
  2. washThe combined organic phases are washed with dilute HCl solution and saturated NaCl solution
  3. filtrationfiltered through a Whatman
  4. filtrationfilter
  5. concentrationconcentrated by evaporation

출처 및 근거

ORD 기록
ord-1a727ba01de04ffa957a0a1c21630526
출처 데이터셋
uspto-grants-2007_12
특허 번호
US07312225B2

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