Water → HCID 57423909, 화합물

HRID 2064064노트

반응식

HRID 2064064 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[C:4](F)[CH:3]=1.[NH2:12][CH:13]1[CH2:18][CH2:17][N:16]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:15][CH2:14]1.O.C(OCC)(=O)C>CN(C)C=O.C(N(C(C)C)CC)(C)C>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[C:4]([NH:12][CH:13]2[CH2:14][CH2:15][N:16]([C:19]([O:21][C:22]([CH3:25])([CH3:24])[CH3:23])=[O:20])[CH2:17][CH2:18]2)[CH:3]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 696914-Chloro-2-fluoro-1-nitrobenzeneHCID 12682914-Amino-1-Boc-piperidine

생성물 1

HCID 57423909HCID 57423909, 화합물

시약·촉매·용매 2

HCID 6228Dimethylformamide용매HCID 81531Diisopropylethylamine용매

반응 조건

온도
80 °C

실험 절차

4-Chloro-2-fluoronitrobenzene (3.5 g) was dissolved in dry dimethylformamide (25 mL) and diisopropylethylamine (3.6 mL), and 1,1-dimethylethyl 4-amino-1-piperidinecarboxylate (4.2 g) were added at room temperature. The mixture was stirred at 80° C. for 1 h, then cooled to room temperature and water and ethyl acetate added. The organic layer was dried over MgSO4, filtered and evaporated, and the residue was purified by chromatography eluting with 10 to 25% ethyl acetate in hexane to afford the title compound, 6.8 g.

후처리

  1. temperaturecooled to room temperature
  2. dry with materialThe organic layer was dried over MgSO4
  3. filtrationfiltered
  4. customevaporated
  5. customthe residue was purified by chromatography
  6. washeluting with 10 to 25% ethyl acetate in hexane

출처 및 근거

ORD 기록
ord-4accc71d8bd24ba390096157ec0131a1
출처 데이터셋
uspto-grants-2012_10
특허 번호
US08288413B2

반응 노트

불러오는 중…