Ethyl Acetate → 1-Ethyl-1-[4-[7-(4-methylphenyl)-3,4-dihydronaphthalene-2-carboxamido]benzyl]perhydroazepinium chloride

HRID 565882노트

반응식

HRID 565882 반응식
[Cl:1][CH2:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10]([C:12]2[CH2:21][CH2:20][C:19]3[C:14](=[CH:15][C:16]([C:22]4[CH:27]=[CH:26][C:25]([CH3:28])=[CH:24][CH:23]=4)=[CH:17][CH:18]=3)[CH:13]=2)=[O:11])=[CH:5][CH:4]=1.[CH2:29]([N:31]1[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33][CH2:32]1)[CH3:30].C(OCC)(=O)C>CN(C=O)C>[Cl-:1].[CH2:29]([N+:31]1([CH2:2][C:3]2[CH:8]=[CH:7][C:6]([NH:9][C:10]([C:12]3[CH2:21][CH2:20][C:19]4[C:14](=[CH:15][C:16]([C:22]5[CH:27]=[CH:26][C:25]([CH3:28])=[CH:24][CH:23]=5)=[CH:17][CH:18]=4)[CH:13]=3)=[O:11])=[CH:5][CH:4]=2)[CH2:37][CH2:36][CH2:35][CH2:34][CH2:33][CH2:32]1)[CH3:30]

참가 물질

5

반응물 3

HCID 8857Ethyl AcetateHCID 5355851-EthylazepaneHCID 18472361N-[4-(chloromethyl)phenyl]-7-(4-methylphenyl)-3,4-dihydronaphthalene-2-carboxamide

생성물 1

HCID 184722571-Ethyl-1-[4-[7-(4-methylphenyl)-3,4-dihydronaphthalene-2-carboxamido]benzyl]perhydroazepinium chloride수율 68.8%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In DMF (3ml) was dissolved N-[4-(chloromethyl)-phenyl]-7-(4-methylphenyl)-3,4-dihydronaphthalene-2-carboxamide (150mg), and to the mixture was added 1-ethylperhydroazepine (98mg). The mixture was stirred at room temperature for 15 hours. To the reaction mixture was added ethyl acetate (100ml), and the resulting precipitate was filtered and recrystallized from ethylacetate-methanol to give 1-ethyl-1-[4-[7-(4-methyl-phenyl)-3,4-dihydronaphthalene-2-carboxamido]benzyl]perhydro-azepinium chloride (Compound 37) (137mg) as colorless crystals.

후처리

  1. filtrationthe resulting precipitate was filtered
  2. customrecrystallized from ethylacetate-methanol

출처 및 근거

ORD 기록
ord-10cc66a9fd0f4293a6b820d676cca7d4
출처 데이터셋
uspto-grants-2001_01
특허 번호
US06172061B2

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