N-Methylpiperidine → 1-Methyl-1-(4-((7-(4-methylphenyl)-1,2,3,4-tetrahydroisoquinolin-2-yl)carbonylamino)benzyl)piperidinium chloride

HRID 1169368노트

반응식

HRID 1169368 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][N:14]([C:18]([NH:20][C:21]4[CH:28]=[CH:27][C:24]([CH2:25][Cl:26])=[CH:23][CH:22]=4)=[O:19])[CH2:15]3)=[CH:10][CH:9]=2)=[CH:4][CH:3]=1.[CH3:29][N:30]1[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]1>CN(C)C=O>[Cl-:26].[CH3:29][N+:30]1([CH2:25][C:24]2[CH:27]=[CH:28][C:21]([NH:20][C:18]([N: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)[CH2:15]3)=[O:19])=[CH:22][CH:23]=2)[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]1

참가 물질

4

반응물 2

HCID 12291N-MethylpiperidineHCID 229900814-(7-(4-Methylphenyl)-1,2,3,4-tetrahydroisoquinolin-2-ylcarbonylamino)benzyl chloride

생성물 1

HCID 229899451-Methyl-1-(4-((7-(4-methylphenyl)-1,2,3,4-tetrahydroisoquinolin-2-yl)carbonylamino)benzyl)piperidinium chloride

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 4-(7-(4-methylphenyl)-1,2,3,4-tetrahydroisoquinolin-2-ylcarbonylamino)benzyl chloride (0.2 g) and 1-methyl piperidine (0.19 ml) in dimethylformamide (5 ml) was stirred overnight at room temperature under a nitrogen atmosphere. The reaction mixture was evaporated to remove the solvent and was mixed with ethyl acetate, and the precipitate was collected by filtration. The precipitate was recrystallized from ethanol to obtain 1-methyl-1-(4-((7-(4-methylphenyl)-1,2,3,4-tetrahydroisoquinolin-2-yl)carbonylamino)benzyl)piperidinium chloride (compound 29) (0.23 g) as colorless crystals.

후처리

  1. customThe reaction mixture was evaporated
  2. customto remove the solvent
  3. additionwas mixed with ethyl acetate
  4. filtrationthe precipitate was collected by filtration
  5. customThe precipitate was recrystallized from ethanol

출처 및 근거

ORD 기록
ord-e13bc54846ba494da91abd93dd712e89
출처 데이터셋
uspto-grants-2003_09
특허 번호
US06627651B1

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