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

HRID 1004727ノート

反応式

HRID 1004727 の反応式
[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]

参加物

6

反応物 3

HCID 24758Sodium hydrideHCID 178730Furan, 2-chlorotetrahydro-HCID 15389820HCID 15389820、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-edd4e1fcd2a14d3e81a0c92b3e5274e5
出典データセット
uspto-grants-2000_04
特許番号
US06051678

反応ノート

読み込み中…