Tetrahydrofuran → Diethyl vinyl phosphate

HRID 1464864

반응식

HRID 1464864 반응식
[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]

참가 물질

4

반응물 3

HCID 8028TetrahydrofuranHCID 13139Diethyl chlorophosphateHCID 61028n-Butyl lithium

생성물 1

HCID 573017Diethyl vinyl phosphate

반응 조건

온도
0 °C

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-b51dc8cbfe264b779b9b095261875fe1
출처 데이터셋
uspto-grants-2015_04
특허 번호
US08999323B2

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