Sodium hydride → Oxolan-2-yl 1-ethenyl-2-oxopyrrolidine-3-carboxylate

HRID 1004727노트

반응식

HRID 1004727 반응식
[C:1]([O:5][C:6]([CH:8]1[CH2:12][CH2:11][N:10]([CH:13]=[CH2:14])[C:9]1=[O:15])=[O:7])([CH3:4])(C)C.[H-].[Na+].Cl[CH:19]1[CH2:23]CC[O:20]1>O1CCCC1.C(OCC)C>[O:20]1[CH2:19][CH2:23][CH2:4][CH:1]1[O:5][C:6]([CH:8]1[CH2:12][CH2:11][N:10]([CH:13]=[CH2:14])[C:9]1=[O:15])=[O:7]

참가 물질

6

반응물 3

HCID 24758Sodium hydrideHCID 178730Furan, 2-chlorotetrahydro-HCID 15389820HCID 15389820, 화합물

생성물 1

HCID 54014762Oxolan-2-yl 1-ethenyl-2-oxopyrrolidine-3-carboxylate수율 100%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 8028Tetrahydrofuran용매

실험 절차

8.9 g of 3-(t-butoxycarbonyl)-1-vinyl-2-pyrrolidinone (BCVP) was dissolved in 50 ml of tetrahydrofuran free of moisture. To this solution 1.0 g of sodium hydride and 4.4 g of 2-chlorotetrahydrofuran were added and allowed to react at room temperature for 1 hour. This solution was diluted with diethylether and washed many times with pure water. The organic solvent of the organic phase was evaporated and the residue was subjected to silica gel column chromatography, to obtain 9.3 g of pure 3-(tetrahydrofuranyloxycarbonyl)-1-vinyl-2-pyrrolidinone (hereinafter referred to as "TFVP"). Its chemical structure was determined by IR spectra and NMR.

후처리

  1. customto react at room temperature for 1 hour
  2. washwashed many times with pure water
  3. customThe organic solvent of the organic phase was evaporated

출처 및 근거

ORD 기록
ord-edd4e1fcd2a14d3e81a0c92b3e5274e5
출처 데이터셋
uspto-grants-2000_04
특허 번호
US06051678

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