Methanol → HCID 69157076、化合物

HRID 750155ノート

反応式

HRID 750155 の反応式
[CH3:1][O:2][C:3]([C:5]1[N:6]([CH2:23][C:24]2[CH:32]=[CH:31][C:27]3[O:28][CH2:29][O:30][C:26]=3[CH:25]=2)[C:7](=[O:22])[C:8]2[C:13]([C:14]=1[C:15]1[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=1)=[CH:12][C:11](Br)=[CH:10][CH:9]=2)=[O:4].CO.[H][H]>[C].[Pd].C1COCC1>[CH3:1][O:2][C:3]([C:5]1[N:6]([CH2:23][C:24]2[CH:32]=[CH:31][C:27]3[O:28][CH2:29][O:30][C:26]=3[CH:25]=2)[C:7](=[O:22])[C:8]2[C:13]([C:14]=1[C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1)=[CH:12][CH:11]=[CH:10][CH:9]=2)=[O:4]

参加物

6

反応物 3

HCID 887MethanolHCID 10239063HCID 10239063、化合物HCID 178418361HCID 178418361、化合物

生成物 1

HCID 69157076HCID 69157076、化合物収率 91.3%

試薬・触媒・溶媒 2

HCID 178418390HCID 178418390、化合物触媒HCID 8028Tetrahydrofuran溶媒

実験手順

A mixture of 2-benzo[1,3]dioxol-5-ylmethyl-6-bromo-1-oxo-4-phenyl-1,2-dihydroisoquinoline-3-carboxylic acid methyl ester (300 mg), 10% palladium carbon (300 mg), methanol (6 ml) and THF (6 ml) was stirred at room temperature under 1 atm hydrogen pressure for 12 hrs. Palladium carbon was filtered off, and the filtrate was concentrated. The residue was purified by silica gel column chromatography (ethyl acetate) and recrystallized (ethyl acetate-hexane) to give the title compound (230 mg).

後処理

  1. filtrationPalladium carbon was filtered off
  2. concentrationthe filtrate was concentrated
  3. customThe residue was purified by silica gel column chromatography (ethyl acetate)
  4. customrecrystallized (ethyl acetate-hexane)

出典と根拠

ORDレコード
ord-6c90fd2a94f947228e7f33d246a84403
出典データセット
uspto-grants-2008_07
特許番号
US07402595B2

反応ノート

読み込み中…