Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl ester → Ethyl 9-cyanonon-2-enoate

HRID 441534ノート

反応式

HRID 441534 の反応式
[C:1]([CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH:9]=O)#[N:2].C1(P(=[CH:30][C:31]([O:33][CH2:34][CH3:35])=[O:32])(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1C=CC=CC=1>[CH2:34]([O:33][C:31](=[O:32])[CH:30]=[CH:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][C:1]#[N:2])[CH3:35]

参加物

4

反応物 2

HCID 70670Acetic acid, 2-(triphenylphosphoranylidene)-, ethyl esterHCID 109205897-CYANOHEPTANAL

生成物 1

HCID 54099068Ethyl 9-cyanonon-2-enoate

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

The starting material is prepared as follows: The mixture of 14 g of 7-cyanoheptanal, 38 g of ethyl triphenylphosphoranylidene-acetate and 100 ml of benzene is refluxed for 15 hours and evaporated. The residue is triturated with diethyl ether, filtered and the filtrate evaporated. The residue is allowed to stand overnight in the refrigerator, triturated with the minimum amount of diethyl ether, the suspension filtered, the filtrate evaporated, the residue distilled and the fraction boiling at 130°-138° /0.1 mm Hg collected, to yield the 9-cyano-2-nonenoic acid ethyl ester of the formula

後処理

  1. customThe starting material is prepared
  2. temperatureis refluxed for 15 hours
  3. customevaporated
  4. customThe residue is triturated with diethyl ether
  5. filtrationfiltered
  6. customthe filtrate evaporated
  7. customtriturated with the minimum amount of diethyl ether
  8. filtrationthe suspension filtered
  9. customthe filtrate evaporated
  10. distillationthe residue distilled
  11. customthe fraction boiling at 130°-138° /0.1 mm Hg collected

出典と根拠

ORDレコード
ord-8b6ab8b07c454e549f2c999ed71ae819
出典データセット
uspto-grants-1977_08
特許番号
US04041047

反応ノート

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