Tetrahydrofuran → Diethyl vinyl phosphate

HRID 1464864

反応式

HRID 1464864 の反応式
[Li+].CCC[CH2-].Cl[P:7](=[O:14])([O:11][CH2:12][CH3:13])[O:8][CH2:9][CH3:10].[CH2:15]1[CH2:19][O:18]CC1>>[P:7]([O:18][CH:19]=[CH2:15])([O:11][CH2:12][CH3:13])([O:8][CH2:9][CH3:10])=[O:14]

参加物

4

反応物 3

HCID 8028TetrahydrofuranHCID 13139Diethyl chlorophosphateHCID 61028n-Butyl lithium

生成物 1

HCID 573017Diethyl vinyl phosphate

反応条件

温度
0 °C

実験手順

10 ml of N-butyllithium solution (2.1 M solution in hexane) were added dropwise to 50 ml of abs. THF under an argon atmosphere at 0° C. The solution was stirred for 30 minutes at 0° C. and for 15 hours at room temperature, then added to 3.01 ml diethyl chlorophosphonate (20 mmol) at −76° C. and stirred for 1 h at 0° C., then for 16 hours at room temperature. A white solid was filtered off, and the solvent was removed on a rotary evaporator. The slightly yellowish crude product was purified by column chromatography on silica gel (PE:EE=4:1). 2.2 g (60% of th.) of the title compound were obtained as a yellowish liquid.

後処理

  1. customat 0° C
  2. stirringstirred for 1 h at 0° C.
  3. waitfor 16 hours at room temperature
  4. filtrationA white solid was filtered off
  5. customthe solvent was removed on a rotary evaporator
  6. customThe slightly yellowish crude product was purified by column chromatography on silica gel (PE:EE=4:1)

出典と根拠

ORDレコード
ord-b51dc8cbfe264b779b9b095261875fe1
出典データセット
uspto-grants-2015_04
特許番号
US08999323B2

関連ノート

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