Methane → 3,4,5-Trimethoxyhydrocinnamic acid

HRID 990307

반응식

HRID 990307 반응식
[C:1](=[O:4])([O-])[O-:2].[K+].[K+].[CH3:7][O:8][C:9]1[CH:10]=[C:11]([C:19](=C)[C:20](O)=O)[CH:12]=[C:13]([O:17][CH3:18])[C:14]=1[O:15][CH3:16].C>[Pd].O>[CH3:18][O:17][C:13]1[CH:12]=[C:11]([CH2:19][CH2:20][C:1]([OH:2])=[O:4])[CH:10]=[C:9]([O:8][CH3:7])[C:14]=1[O:15][CH3:16]

참가 물질

6

반응물 3

HCID 297MethaneHCID 11430Potassium CarbonateHCID 208491922-(3,4,5-Trimethoxyphenyl)prop-2-enoic acid

생성물 1

HCID 648603,4,5-Trimethoxyhydrocinnamic acid수율 167.5%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 962Water용매

실험 절차

6.8 g of potassium carbonate is added to a solution of 21.44 g of 3,4,5-trimethoxyphenylpropenoic acid and 45 ml of water then the medium is hydrogenated for one hour under a pressure of 1200-1300 mbars in the presence of 1.8 g activated charcoal with 10% palladium, in this way 2.1 l of hydrogen is absorbed. The reaction medium is filtered, followed by washing with water and acidifying with 50 ml of hydrochloric acid (2N). After separation, the residue is washed with water and dried under reduced pressure at ambient temperature. In this way 19.8 g of the expected product is obtained (M.P.=102-103° C.)

후처리

  1. customin this way 2.1 l of hydrogen is absorbed
  2. filtrationThe reaction medium is filtered
  3. washby washing with water and acidifying with 50 ml of hydrochloric acid (2N)
  4. customAfter separation
  5. washthe residue is washed with water
  6. customdried under reduced pressure at ambient temperature

출처 및 근거

ORD 기록
ord-1520d5cc440741be96bb0ab6200a861d
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06459001B1

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