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Benzene → (E)-ethyl 7-hydroxy-2-methyl-2-heptenate

HRID 1433236
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HRID 1433236 반응식
[O:1]1[CH2:6][CH2:5][CH2:4][CH2:3][CH:2]1[OH:7].C([O:10][C:11]([CH2:13][CH:14]=[C:15]1CCP(C2C=CC=CC=2)C1(C1C=CC=CC=1)C1C=CC=CC=1)=O)C.[CH:38]1C=CC=CC=1>>[OH:10][CH2:11][CH2:13][CH2:14][CH2:15]/[CH:4]=[C:3](\[CH3:38])/[C:2]([O:1][CH2:6][CH3:5])=[O:7]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 3

HCID 241BenzeneHCID 1365052-HydroxytetrahydropyranHCID 67123092(Ethoxycarbonylethylidene) triphenylphospholane

생성물 1

HCID 10559469(E)-ethyl 7-hydroxy-2-methyl-2-heptenate

반응 조건

온도
90 °C

실험 절차

Tetrahydropyran-2-ol (2) (14.03 g; 0.138 mol) is added to a benzene solution (300 ml) of (ethoxycarbonylethylidene) triphenylphospholane (64.40 g; 0.178 mol) and the whole is refluxed at 90° C. for 1.5 hours. After the temperature is returned to room temperature, the solvent is then distilled off under reduced pressure, and the residue is separated and purified by column chromatography (developing solution, ethyl acetate:hexane=1:5) to produce Ester 3 (25.15 g; 0.135 mol) of 98% in yield.

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

후처리

  1. customis returned to room temperature
  2. distillationthe solvent is then distilled off under reduced pressure
  3. customthe residue is separated
  4. custompurified by column chromatography (developing solution, ethyl acetate:hexane=1:5)

출처 및 근거

ORD 기록
ord-8e7b9e4d23c445d28adf2736c0f1a1ef
출처 데이터셋
uspto-grants-2009_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07612213B2

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