Ammonia → 1-(tert-Butoxycarbonyl)piperidine-4-carboxamide

HRID 1351413노트

반응식

HRID 1351413 반응식
ClC(OCC)=O.[C:7]([O:11][C:12]([N:14]1[CH2:19][CH2:18][CH:17]([C:20]([OH:22])=O)[CH2:16][CH2:15]1)=[O:13])([CH3:10])([CH3:9])[CH3:8].C([N:25](CC)CC)C.N>ClCCl>[NH2:25][C:20]([CH:17]1[CH2:18][CH2:19][N:14]([C:12]([O:11][C:7]([CH3:10])([CH3:9])[CH3:8])=[O:13])[CH2:15][CH2:16]1)=[O:22]

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 8471TriethylamineHCID 10928Ethyl chloroformateHCID 3928711-(tert-Butoxycarbonyl)-4-piperidinecarboxylic acid

생성물 1

HCID 27356461-(tert-Butoxycarbonyl)piperidine-4-carboxamide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

Ethyl chloroformate (4.6 ml, 48.3 mmol) was added slowly to a solution of 1-(tert-butoxycarbonyl)4-piperidinecarboxylic acid (10 g, 43.6 mmol) in dichloromethane (100 ml) stirred at 0° C. Triethylamine (7.6 ml, 52.3 mmol) was added with stirring over two minutes. 0.88 Ammonia solution (40 ml) was added and the mixture allowed to warm to room temperature with stirring. The mixture was washed with water, 1M citric acid solution and brine, dried (MgSO4), filtered and evaporated under reduced pressure gave the title compound as white solid, 8.94 g.

후처리

  1. stirringwith stirring over two minutes
  2. temperatureto warm to room temperature
  3. stirringwith stirring
  4. washThe mixture was washed with water, 1M citric acid solution and brine
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. customevaporated under reduced pressure

출처 및 근거

ORD 기록
ord-e92e786ce4ae406fadd39dc142270641
출처 데이터셋
uspto-grants-2007_05
특허 번호
US07217714B1

반응 노트

불러오는 중…