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Ammonia → HCID 25184774, 화합물

HRID 1878069
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반응식

HRID 1878069 반응식
[Cl:1][CH2:2][C:3]([NH:5][C:6]1[CH:7]=[N:8][C:9]([C:12](=[N:14][OH:15])[NH2:13])=[CH:10][CH:11]=1)=[O:4].N.[Cl:17][CH2:18][C:19](Cl)=O>>[Cl:1][CH2:2][C:3]([NH:5][C:6]1[CH:7]=[N:8][C:9]([C:12]2[N:13]=[C:19]([CH2:18][Cl:17])[O:15][N:14]=2)=[CH:10][CH:11]=1)=[O:4]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 222AmmoniaHCID 6577Chloroacetyl chlorideHCID 137068883HCID 137068883, 화합물

생성물 1

HCID 25184774HCID 25184774, 화합물

실험 절차

Compound of example 4 (0.500 g, 2.18 mmol) was heated in chloroacetyl chloride (2 mL) at a temperature in the range of 100-110° C. for 4 hours. The reaction mixture was cooled, poured over ice water, basified With ammonia solution, and extracted with ethyl acetate (3×60 mL). The organic layer was washed with brine, dried over sodium sulfate and concentrated. The crude product obtained was purified over silica gel using ethyl acetate/petroleum ether (35%-50%) as eluent, and the pure fractions were concentrated and crystallized using chloroform/ petroleum ether, to obtain the title compound.

후처리

  1. temperatureThe reaction mixture was cooled
  • extractionextracted with ethyl acetate (3×60 mL)
  • washThe organic layer was washed with brine
  • dry with materialdried over sodium sulfate
  • concentrationconcentrated
  • customThe crude product obtained
  • customwas purified over silica gel
  • concentrationthe pure fractions were concentrated
  • customcrystallized
  • 출처 및 근거

    ORD 기록
    ord-e4f28d44955348299df5bd33dfefcc4e
    출처 데이터셋
    uspto-grants-2012_11
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US08314103B2

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