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

HRID 918279노트

반응식

HRID 918279 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 54099068Ethyl 9-cyanonon-2-enoate

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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

후처리

  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

출처 및 근거

ORD 기록
ord-dae1e7e5169741cfaab22c2d0f6dede9
출처 데이터셋
uspto-grants-1976_07
특허 번호
US03970670

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