Ethyl Bromide → Triethyl 4-phosphonocrotonate, mixture of isomers

HRID 333040ノート

反応式

HRID 333040 の反応式
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]

参加物

4

反応物 3

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

生成物 1

HCID 5365783Triethyl 4-phosphonocrotonate, mixture of isomers

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-1b7724c1078e4691bfc77b728110268c
出典データセット
uspto-grants-2014_11
特許番号
US08877953B2

反応ノート

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