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Water → HCID 13712178, 화합물

HRID 414048
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HRID 414048 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8](Cl)(=[O:10])=[O:9])=[CH:4][CH:3]=1.[CH3:12][NH:13][CH2:14][CH2:15][NH:16][CH3:17].C(=O)([O-])[O-].[Na+].[Na+].O>C(Cl)(Cl)Cl>[F:1][C:2]1[CH:7]=[CH:6][C:5]([S:8]([N:13]([CH3:12])[CH2:14][CH2:15][NH:16][CH3:17])(=[O:10])=[O:9])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 8070N,N'-DimethylethylenediamineHCID 95884-Fluorobenzenesulfonyl chlorideHCID 10340Sodium Carbonate

생성물 1

HCID 13712178HCID 13712178, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매4회

실험 절차

A solution of 4-fluorobenzenesulphonyl chloride (6.0 g) in chloroform (30 ml) was added dropwise to a well-stirred solution of N,N'-dimethyl-ethylenediamine (25 g) in chloroform (300 ml) at room temperature. After 2 hours the chloroform solution was vigorously shaken with aqueous sodium carbonate solution, separated, dried (MgSO4) and evaporated under reduced pressure to give an oil. The oil was treated with chloroform (60 ml) and water (100 ml). The two solvents were mixed thoroughly and were then separated. The chloroform layer was dried (MgSO4) and evaporated under reduced pressure to give an oil. Final traces of N,N'-dimethyl-ethylenediamine were removed by heating the oil under low vacuum to give 4-fluoro-N-methyl-N-[2-(methylamino)ethyl]benzenesulphonamide.

후처리

  1. customseparated
  2. dry with materialdried (MgSO4)
  3. customevaporated under reduced pressure
  4. customto give an oil
  5. additionThe two solvents were mixed thoroughly
  6. customwere then separated
  7. dry with materialThe chloroform layer was dried (MgSO4)
  8. customevaporated under reduced pressure
  9. customto give an oil
  10. customFinal traces of N,N'-dimethyl-ethylenediamine were removed
  11. temperatureby heating the oil under low vacuum

출처 및 근거

ORD 기록
ord-462fd15b02c54a828f05357b256871a0
출처 데이터셋
uspto-grants-1988_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04789677

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