Ammonia → HCID 178420422, 화합물

HRID 333749

반응식

HRID 333749 반응식
[CH2:1]([O:8][CH2:9][CH2:10][CH2:11][C:12](O)=O)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[NH2:15][C:16]1[C:21]([NH2:22])=[CH:20][CH:19]=[CH:18][N:17]=1.N>>[CH2:1]([O:8][CH2:9][CH2:10][CH2:11][C:12]1[NH:15][C:16]2=[N:17][CH:18]=[CH:19][CH:20]=[C:21]2[N:22]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 3

HCID 222AmmoniaHCID 99562,3-DiaminopyridineHCID 5622014-(Benzyloxy)butanoic acid

생성물 1

HCID 178420422HCID 178420422, 화합물수율 86%

실험 절차

4-(Benzyloxy)butanoic acid (5.0 g) and 2,3-diaminopyridine (1.12 g) were stirred at 150° C. for 10 hr. Under ice-cooling, to the reaction mixture was added concentrated aqueous ammonia, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (2.36 g).

후처리

  1. temperatureUnder ice-cooling, to the reaction mixture
  2. extractionthe mixture was extracted with ethyl acetate
  3. washThe organic layer was washed with saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-257fd407c9e749c5858e8bd50352b094
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08883788B2

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