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Methane → 3,4,5-Trimethoxyhydrocinnamic acid

HRID 325022
ノート
印刷プレビュー

反応式

HRID 325022 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

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

生成物 1

HCID 648603,4,5-Trimethoxyhydrocinnamic acid収率 167.5%

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 962Water溶媒

実験手順

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.).

後処理

  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

出典と根拠

ORDレコード
ord-8cc873cd4ee7468f94dde1f576824c0e
出典データセット
uspto-grants-2001_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06221907B1

反応ノート

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