Acetic acid, 2-(triphenylphosphoranylidene)-, methyl ester → HCID 86737542、化合物

HRID 126997

反応式

HRID 126997 の反応式
[C:1]([CH:5]=P(C1C=CC=CC=1)(C1C=CC=CC=1)C1C=CC=CC=1)([O:3][CH3:4])=[O:2].Br[CH2:26][C:27]([C:29]1[CH:34]=[CH:33][CH:32]=[CH:31][N:30]=1)=[O:28]>C1C=CC=CC=1>[N:30]1[CH:31]=[CH:32][CH:33]=[CH:34][C:29]=1[C:27](=[O:28])[CH:26]=[CH:5][C:1]([O:3][CH3:4])=[O:2]

参加物

4

反応物 2

HCID 17453Acetic acid, 2-(triphenylphosphoranylidene)-, methyl esterHCID 383842-Bromoacetamidopyridine

生成物 1

HCID 86737542HCID 86737542、化合物

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A solution of 33.4 g of carbomethoxymethylene triphenylphosphine [Helv. Chim. Acta. 40, 1242 (1957)] in 500 ml of dry benzene under nitrogen is treated with 10 g of 2-(bromoacetyl)pyridine and heated at reflux temperature for 2 hours. The reaction mixture is cooled and filtered to remove carbomethoxymethyl triphenylphosphonium bromide. The filtrate, containing triphenylphosphine, is treated with methyl bromoacetate and heated at reflux temperature for 2 hours. Cooling and filtration removes additional phosphonium salt. The filtrate is concentrated in vacuo yielding the title compound.

後処理

  1. temperatureheated
  2. temperatureat reflux temperature for 2 hours
  3. temperatureThe reaction mixture is cooled
  4. filtrationfiltered
  5. customto remove carbomethoxymethyl triphenylphosphonium bromide
  6. additionThe filtrate, containing triphenylphosphine
  7. additionis treated with methyl bromoacetate
  8. temperatureheated
  9. temperatureat reflux temperature for 2 hours
  10. temperatureCooling
  11. filtrationfiltration
  12. customremoves additional phosphonium salt
  13. concentrationThe filtrate is concentrated in vacuo

出典と根拠

ORDレコード
ord-9a5a6a6380dd44f8a41023491fe93aa0
出典データセット
uspto-grants-1981_03
特許番号
US04254267

関連ノート

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