Ethyl Bromide → Triethyl 4-phosphonocrotonate, mixture of isomers

HRID 333040노트

반응식

HRID 333040 반응식
Br[CH2:2]/[CH:3]=[CH:4]/[C:5]([O:7][CH2:8][CH3:9])=[O:6].[CH2:10]([O:12][P:13]([O:17]CC)[O:14][CH2:15][CH3:16])[CH3:11].C(Br)C>>[CH3:9][CH2:8][O:7][C:5](/[CH:4]=[CH:3]/[CH2:2][P:13]([O:14][CH2:15][CH3:16])([O:12][CH2:10][CH3:11])=[O:17])=[O:6]

참가 물질

4

반응물 3

HCID 6332Ethyl BromideHCID 31215Triethyl phosphiteHCID 5373944Ethyl (E)-4-bromobut-2-enoate

생성물 1

HCID 5365783Triethyl 4-phosphonocrotonate, mixture of isomers

실험 절차

Ethyl 4-bromocrotonate (7.0 mL) was added to triethylphosphite (9.9 mL) at 120 to 130° C. during 60 minutes periods. After the generation of ethyl bromide ceased, the reaction solution was stirred at the same temperature for 3 hours. After cooling, the resulting reaction solution was concentrated under reduced pressure. Then the residue was purified by distillation at 150 to 210° C. under reduced pressure (17 to 21 hPa) to give triethyl 4-phosphonocrotonate as colorless oil.

후처리

  1. temperatureAfter cooling
  2. customthe resulting reaction solution
  3. concentrationwas concentrated under reduced pressure
  4. distillationThen the residue was purified by distillation at 150 to 210° C. under reduced pressure (17 to 21 hPa)

출처 및 근거

ORD 기록
ord-1b7724c1078e4691bfc77b728110268c
출처 데이터셋
uspto-grants-2014_11
특허 번호
US08877953B2

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