Ethyl [(phenoxycarbonyl)oxy]acetate → 2-(Ethyloxy)-2-oxoethyl 4-[(4-bromophenyl)oxy]-1-piperidinecarboxylate

HRID 2242933노트

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HRID 2242933 반응식
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH:9]2[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]2)=[CH:4][CH:3]=1.C1([O:21][C:22]([O:24][CH2:25][C:26]([O:28][CH2:29][CH3:30])=[O:27])=O)C=CC=CC=1>C1(C)C=CC=CC=1>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][CH:9]2[CH2:14][CH2:13][N:12]([C:22]([O:24][CH2:25][C:26]([O:28][CH2:29][CH3:30])=[O:27])=[O:21])[CH2:11][CH2:10]2)=[CH:4][CH:3]=1

참가 물질

4

반응물 2

HCID 12094709Ethyl [(phenoxycarbonyl)oxy]acetateHCID 126455664-(4-Bromophenoxy)piperidine

생성물 1

HCID 674168332-(Ethyloxy)-2-oxoethyl 4-[(4-bromophenyl)oxy]-1-piperidinecarboxylate수율 99.1%

시약·촉매·용매 1

HCID 1140Toluene용매

반응 조건

온도
50 °C

실험 절차

2.7 g (7.58 mmol) of 4-[(4-bromophenyl)-oxy]piperidine, prepared in Step 4.2, and 1.70 g (7.6 mmol) of ethyl {[(phenyloxy)carbonyl]oxy}acetate, prepared in accordance with Example 1.1, are mixed in 40 ml of toluene and the solution is heated at 50° C. for 20 hours. After cooling, it is evaporated to dryness and the product is purified by chromatography on silica gel, eluting with a 40/60 mixture of ethyl acetate and cyclohexane. The eluate is subsequently triturated in diisopropyl ether, to give 2.9 g of product in powder form.

후처리

  1. customprepared in accordance with Example 1.1
  2. temperatureAfter cooling
  3. customit is evaporated to dryness
  4. customthe product is purified by chromatography on silica gel
  5. washeluting with a 40/60 mixture of ethyl acetate and cyclohexane
  6. customThe eluate is subsequently triturated in diisopropyl ether

출처 및 근거

ORD 기록
ord-81afad4f08c84058abee8c63369f8144
출처 데이터셋
uspto-grants-2010_03
특허 번호
US07674805B2

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