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Sodium Carbonate → Benzyl 4-(2-ethoxy-2-oxoethyl)piperidine-1-carboxylate

HRID 1664777
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인쇄 미리보기

반응식

HRID 1664777 반응식
[CH:1]1[CH:6]=[CH:5][C:4]([CH2:7][O:8][C:9](Cl)=[O:10])=[CH:3][CH:2]=1.[NH:12]1[CH2:17][CH2:16][CH:15]([CH2:18][C:19]([O:21][CH2:22][CH3:23])=[O:20])[CH2:14][CH2:13]1.C(=O)([O-])[O-].[Na+].[Na+]>ClCCl>[CH2:22]([O:21][C:19](=[O:20])[CH2:18][CH:15]1[CH2:16][CH2:17][N:12]([C:9]([O:8][CH2:7][C:4]2[CH:5]=[CH:6][CH:1]=[CH:2][CH:3]=2)=[O:10])[CH2:13][CH2:14]1)[CH3:23]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 10340Sodium CarbonateHCID 10387Benzyl chloroformateHCID 2760465Ethyl 2-(piperidin-4-yl)acetate

생성물 1

HCID 12902702Benzyl 4-(2-ethoxy-2-oxoethyl)piperidine-1-carboxylate수율 98.7%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Benzyl chloridocarbonate (10.5 g, 61.3 mmol) was added to a solution of ethyl piperidin-4-ylacetate (10.0 g, 58.4 mmol) and sodium carbonate (46.2 g, 438 mmol) in dichloromethane (320 mL). After 18 h, the reaction mixture was filtered and concentrated. Purification by silica gel chromatography [75% hexanes/ethyl acetate→50% hexanes/ethyl acetate)] gave the title compound (17.6 g). MS 306.1 (M+1).

후처리

  1. filtrationthe reaction mixture was filtered
  2. concentrationconcentrated
  3. customPurification by silica gel chromatography [75% hexanes/ethyl acetate→50% hexanes/ethyl acetate)]

출처 및 근거

ORD 기록
ord-be89863e21194506a79c87ed733f6e0f
출처 데이터셋
uspto-grants-2011_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08039460B2

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