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7-Methoxy-3,7-Dimethyloctanal → HCID 53925657, 화합물

HRID 1658874
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HRID 1658874 반응식
[CH3:1][CH:2]([CH2:6][CH2:7][CH2:8][C:9]([CH3:13])([O:11][CH3:12])[CH3:10])[CH2:3][CH:4]=O.[CH3:14][O:15][C:16](=[O:29])/[C:17](/[CH3:28])=[C:18](\P(OCC)(OCC)=O)/[CH3:19].[Na]>C1C=CC=CC=1.CO>[CH3:14][O:15][C:16](=[O:29])[C:17]([CH3:28])=[CH:18][CH:19]=[CH:4][CH2:3][CH:2]([CH3:1])[CH2:6][CH2:7][CH2:8][C:9]([O:11][CH3:12])([CH3:13])[CH3:10]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 192237-Methoxy-3,7-DimethyloctanalHCID 5360545SodiumHCID 86733613HCID 86733613, 화합물

생성물 1

HCID 53925657HCID 53925657, 화합물

시약·촉매·용매 2

HCID 241Benzene용매HCID 887Methanol용매

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온도
60 °C

실험 절차

29.5 g of 3,7-dimethyl-7-methoxy-octanal and 42 g of diethylphosphono-α-methyl-crotonic acid methyl ester are dissolved in 100 ml of absolute benzene. To this solution there is added dropwise 4.1 g of sodium dissolved in 50 ml of absolute methanol. The mixture is stirred for 5 hours at 60°C., poured on to ice-water and extracted with diethyl ether. The ethereal solution is washed with water, then with aqueous sodium bicarbonate solution and once again with water, dried with sodium sulphate, filtered and concentrated on a rotary evaporator. After chromatography on a 30-fold amount of Kieselgel, using hexane/diethyl ether (9:1 parts by volume) as the eluant, there is obtained 11-methoxy-2,7,11-trimethyl-2,4-dodecadienoic acid methyl ester; boiling point 100°C/0.002 mmHg.

후처리

  1. extractionextracted with diethyl ether
  2. washThe ethereal solution is washed with water
  3. dry with materialwith aqueous sodium bicarbonate solution and once again with water, dried with sodium sulphate
  4. filtrationfiltered
  5. concentrationconcentrated on a rotary evaporator

출처 및 근거

ORD 기록
ord-6cdc5275c9c442d39ca810b19e17710d
출처 데이터셋
uspto-grants-1976_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03966780

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