Chloroform → Benzyl 4-(3-ethoxy-3-oxopropyl)piperidine-1-carboxylate

HRID 1195661노트

반응식

HRID 1195661 반응식
[C:1]1([CH2:7][O:8][C:9](Cl)=[O:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[NH:12]1[CH2:17][CH2:16][CH:15]([CH2:18][CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[CH2:14][CH2:13]1.C(=O)([O-])[O-].[Na+].[Na+].ClC(Cl)Cl>O>[C:1]1([CH2:7][O:8][C:9]([N:12]2[CH2:17][CH2:16][CH:15]([CH2:18][CH2:19][C:20]([O:22][CH2:23][CH3:24])=[O:21])[CH2:14][CH2:13]2)=[O:10])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

참가 물질

6

반응물 4

HCID 6212ChloroformHCID 10340Sodium CarbonateHCID 10387Benzyl chloroformateHCID 10012639Ethyl 3-piperidin-4-ylpropanoate

생성물 1

HCID 14989191Benzyl 4-(3-ethoxy-3-oxopropyl)piperidine-1-carboxylate수율 74%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 54 parts of (phenylmethyl)carbonochloridate, 60 parts of ethyl 4-piperidinepropanoate, 31.8 parts of sodium carbonate and 600 parts of trichloromethane was stirred overnight at room temperature. Water was added and the layers were separated. The organic layer was dried, filtered and evaporated. The residue was purified by filtration over silica gel using a mixture of trichloromethane and methanol (99:1 by volume) as eluent. The pure fractions were collected and the eluent was evaporated, yielding 71 parts (74%) of ethyl 1-(phenylmethoxycarbonyl)-4-piperidinepropanoate as a residue (interm. 1).

후처리

  1. customthe layers were separated
  2. customThe organic layer was dried
  3. filtrationfiltered
  4. customevaporated
  5. filtrationThe residue was purified by filtration over silica gel using
  6. additiona mixture of trichloromethane and methanol (99:1 by volume) as eluent
  7. customThe pure fractions were collected
  8. customthe eluent was evaporated

출처 및 근거

ORD 기록
ord-08ff2416e8c942d3a0575bc504629310
출처 데이터셋
uspto-grants-1992_05
특허 번호
US05112825

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