HCID 69766304, 화합물 → HCID 10404453, 화합물

HRID 966106노트

반응식

HRID 966106 반응식
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

참가 물질

4

반응물 1

HCID 69766304HCID 69766304, 화합물

생성물 1

HCID 10404453HCID 10404453, 화합물수율 64.5%

시약·촉매·용매 2

HCID 345198Adams' catalyst촉매HCID 887Methanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8914d004eec047e09517829430d632a7
출처 데이터셋
uspto-grants-2005_10
특허 번호
US06951888B2

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