Methanol → HCID 10194752, 화합물

HRID 750152노트

반응식

HRID 750152 반응식
[CH3:1][O:2][C:3]([C:5]1[N:6]([CH2:30][C:31]2[CH:39]=[CH:38][C:34]3[O:35][CH2:36][O:37][C:33]=3[CH:32]=2)[C:7](=[O:29])[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]([NH:21]CC1C=CC=CC=1)=[CH:10][CH:9]=2)=[O:4].CO.[H][H]>[C].[Pd].C1COCC1>[CH3:1][O:2][C:3]([C:5]1[N:6]([CH2:30][C:31]2[CH:39]=[CH:38][C:34]3[O:35][CH2:36][O:37][C:33]=3[CH:32]=2)[C:7](=[O:29])[C:8]2[C:13]([C:14]=1[C:15]1[CH:16]=[CH:17][CH:18]=[CH:19][CH:20]=1)=[CH:12][C:11]([NH2:21])=[CH:10][CH:9]=2)=[O:4]

참가 물질

6

반응물 3

HCID 887MethanolHCID 69156557HCID 69156557, 화합물HCID 178418361HCID 178418361, 화합물

생성물 1

HCID 10194752HCID 10194752, 화합물수율 72.3%

시약·촉매·용매 2

HCID 178418390HCID 178418390, 화합물촉매HCID 8028Tetrahydrofuran용매

실험 절차

A mixture of 2-(benzo[1,3]dioxol-5-ylmethyl)-6-benzylamino-1-oxo-4-phenyl-1,2-dihydroisoquinoline-3-carboxylic acid methyl ester (670 mg), 10% palladium carbon (200 mg), methanol (10 ml) and THF (10 ml) was stirred at room temperature at 4-5 atm hydrogen pressure for 48 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 (400 mg).

후처리

  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)

출처 및 근거

ORD 기록
ord-afd71ddd0cb047478987b6584fe942d7
출처 데이터셋
uspto-grants-2008_07
특허 번호
US07402595B2

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