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N,N-Dimethylethylenediamine → 4-(beta-Dimethylaminoethyl)amino-3-nitrophenyl methyl sulfone

HRID 2291969
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HRID 2291969 반응식
[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][C:8](Cl)=[C:7]([N+:12]([O-:14])=[O:13])[CH:6]=1)(=[O:4])=[O:3].[CH3:15][N:16]([CH3:20])[CH2:17][CH2:18][NH2:19]>CS(C)=O>[CH3:1][S:2]([C:5]1[CH:10]=[CH:9][C:8]([NH:19][CH2:18][CH2:17][N:16]([CH3:20])[CH3:15])=[C:7]([N+:12]([O-:14])=[O:13])[CH:6]=1)(=[O:4])=[O:3]
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참가 물질

4

반응물 2

HCID 66053N,N-DimethylethylenediamineHCID 667964-Chloro-3-nitrophenyl methyl sulfone

생성물 1

HCID 212775874-(beta-Dimethylaminoethyl)amino-3-nitrophenyl methyl sulfone수율 78%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

A mixture of 4-chloro-3-nitrophenyl methyl sulfone (4 g, 17 mmole) and N,N-dimethylethylenediamine (3.3 g, 37 mmole) in DMSO (20 ml) was stored at 75° C. for 1 hour and poured into crushed ice. The yellow solid precipitate was collected by filtration and was dissolved in ethyl acetate. The organic phase was washed with water-brine mixture twice and brine, dried over sodium sulfate, and evaporated under reduced pressure to give the sulfone (22) (3.8 g, 78%) as a yellow solid. A pure sample (m.p. 130°-131° C.) was obtained by recrystallization from ethyl acetate.

후처리

  1. additionpoured
  2. custominto crushed ice
  3. filtrationThe yellow solid precipitate was collected by filtration
  4. dissolutionwas dissolved in ethyl acetate
  5. washThe organic phase was washed with water-brine mixture twice
  6. dry with materialbrine, dried over sodium sulfate
  7. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-645817e41c254dacb74297f3f75d2b45
출처 데이터셋
uspto-grants-1989_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04799934

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