Methane → 3,4,5-Trimethoxyhydrocinnamic acid

HRID 619773

반응식

HRID 619773 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.[H][H]>[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

7

반응물 4

HCID 297MethaneHCID 11430Potassium CarbonateHCID 208491922-(3,4,5-Trimethoxyphenyl)prop-2-enoic acidHCID 178418361HCID 178418361, 화합물

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 were added to a solution of 21.44 g of 3,4,5-trimethoxyphenylpropenoic acid and 45 ml of water and the mixture was hydrogenated for one hour under a pressure of 1200-1300 mbar in the presence of 1.8 g of activated charcoal with 10% of palladium during which 2.1 liters of hydrogen were absorbed. Filtration was carried out, followed by washing with water and acidifying with 50 ml of hydrochloric acid (2 N). The product was separated off, washed with water and dried under reduced pressure at ambient temperature to obtain 19.8 g of the expected product melting at 102-103° C.

후처리

  1. customwere absorbed
  2. filtrationFiltration
  3. washby washing with water and acidifying with 50 ml of hydrochloric acid (2 N)
  4. customThe product was separated off
  5. washwashed with water
  6. customdried under reduced pressure at ambient temperature

출처 및 근거

ORD 기록
ord-033cea20126547ecb64b172b41af589d
출처 데이터셋
uspto-grants-1999_09
특허 번호
US05959146

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