HCID 69766304、化合物 → HCID 10404453、化合物

HRID 966106ノート

反応式

HRID 966106 の反応式
Cl.[OH:2][C:3]1[C:4]([O:24][CH3:25])=[C:5]([C:10](=[O:23])[CH2:11][NH:12][C:13]([CH3:22])([CH3:21])[CH2:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[CH:6]=[CH:7][C:8]=1[OH:9]>CO.[Pt](=O)=O>[CH3:22][C:13]([NH:12][CH2:11][CH:10]([C:5]1[C:4]([O:24][CH3:25])=[C:3]([OH:2])[C:8]([OH:9])=[CH:7][CH:6]=1)[OH:23])([CH3:21])[CH2:14][C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1

参加物

4

反応物 1

HCID 69766304HCID 69766304、化合物

生成物 1

HCID 10404453HCID 10404453、化合物収率 64.5%

試薬・触媒・溶媒 2

HCID 345198Adams' catalyst触媒HCID 887Methanol溶媒

実験手順

10 g of 1-(3,4-dihydroxy-2-methoxyphenyl)-2-(1,1-dimethyl-2-phenylethylamino)ethanone hydrochloride is hydrogenated with 0.5 g of platinum(IV) oxide in 200 mL methanol. The catalyst is suction filtered and the solvent is distilled off under reduced pressure. The residue remaining is dissolved in 200 mL acetonitrile, combined with 5 g of sodium benzoate and refluxed for 15 minutes. After the excess sodium benzoate has been filtered off, the product which crystallizes out of the filtrate is filtered off and washed with acetonitrile and diethyl ether. Yield: 64.5% (benzoate); melting point: 149° C.-150° C.

後処理

  1. filtrationfiltered
  2. distillationthe solvent is distilled off under reduced pressure
  3. dissolutionThe residue remaining is dissolved in 200 mL acetonitrile
  4. temperaturerefluxed for 15 minutes
  5. filtrationAfter the excess sodium benzoate has been filtered off
  6. customthe product which crystallizes out of the filtrate
  7. filtrationis filtered off
  8. washwashed with acetonitrile and diethyl ether

出典と根拠

ORDレコード
ord-8914d004eec047e09517829430d632a7
出典データセット
uspto-grants-2005_10
特許番号
US06951888B2

反応ノート

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