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Methyl iodide → 4-Methyl-4-[4-[7-(4-methyl-phenyl)-3,4-dihydronaphthalene-2-carboxamido]benzyl]-thiomorpholinium iodide

HRID 1387831
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HRID 1387831 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:17]=[C:16]3[C:11]([CH2:12][CH2:13][C:14]([C:18]([NH:20][C:21]4[CH:26]=[CH:25][C:24]([CH2:27][N:28]5[CH2:33][CH2:32][S:31][CH2:30][CH2:29]5)=[CH:23][CH:22]=4)=[O:19])=[CH:15]3)=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.C[I:35].[C:36](OCC)(=O)C>CN(C=O)C>[I-:35].[CH3:36][N+:28]1([CH2:27][C:24]2[CH:25]=[CH:26][C:21]([NH:20][C:18]([C:14]3[CH2:13][CH2:12][C:11]4[C:16](=[CH:17][C:8]([C:5]5[CH:4]=[CH:3][C:2]([CH3:1])=[CH:7][CH:6]=5)=[CH:9][CH:10]=4)[CH:15]=3)=[O:19])=[CH:22][CH:23]=2)[CH2:33][CH2:32][S:31][CH2:30][CH2:29]1
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참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 8857Ethyl AcetateHCID 184725127-(4-methylphenyl)-N-[4-(thiomorpholinomethyl)phenyl]-3,4-dihydronaphthalene-2-carboxamide

생성물 1

HCID 184725544-Methyl-4-[4-[7-(4-methyl-phenyl)-3,4-dihydronaphthalene-2-carboxamido]benzyl]-thiomorpholinium iodide

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

In DMF (3 ml) was dissolved 7-(4-methylphenyl)-N-[4-(thiomorpholinomethyl)phenyl]-3,4-dihydronaphthalene-2-carboxamide (160 mg), and to the mixture was added methyl iodide (66 μl). The mixture was stirred at room temperature for 17 hours, and to the mixture was added ethyl acetate (100 ml). The resulting precipitate was filtered and recrystallized from ethyl acetate-methanol to give 4-methyl-4-[4-[7-(4-methyl-phenyl)-3,4-dihydronaphthalene-2-carboxamido]benzyl]-thiomorpholinium iodide (Compound 55) (165 mg) as colorless crystals.

후처리

  1. filtrationThe resulting precipitate was filtered
  2. customrecrystallized from ethyl acetate-methanol

출처 및 근거

ORD 기록
ord-4f781e9dd97b4ee8b68331e92939cc41
출처 데이터셋
uspto-grants-2001_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06268354B1

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