Water → HCID 57423909、化合物

HRID 2064064ノート

反応式

HRID 2064064 の反応式
[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

参加物

7

反応物 4

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

生成物 1

HCID 57423909HCID 57423909、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 81531Diisopropylethylamine溶媒

反応条件

温度
80 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-4accc71d8bd24ba390096157ec0131a1
出典データセット
uspto-grants-2012_10
特許番号
US08288413B2

反応ノート

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