Methyl iodide → HCID 9938497, 화합물

HRID 2228123노트

반응식

HRID 2228123 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[CH:9]=[CH:10][C:11]3[O:17][CH2:16][CH2:15][C:14]([C:18]([NH:20][C:21]4[CH:26]=[CH:25][C:24]([CH2:27][N:28]5[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]5)=[CH:23][CH:22]=4)=[O:19])=[CH:13][C:12]=3[CH:34]=2)=[CH:4][CH:3]=1.[CH3:35][I:36]>CN(C)C=O>[I-:36].[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:9]=[CH:10][C:11]3[O:17][CH2:16][CH2:15][C:14]([C:18]([NH:20][C:21]4[CH:22]=[CH:23][C:24]([CH2:27][N+:28]5([CH3:35])[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]5)=[CH:25][CH:26]=4)=[O:19])=[CH:13][C:12]=3[CH:34]=2)=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 6328Methyl iodideHCID 3013432HCID 3013432, 화합물

생성물 1

HCID 9938497HCID 9938497, 화합물

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

실험 절차

A solution of 7—(4-methylphenyl)-N-(4—(piperidinomethyl)phenyl)-2,3-dihydro-1-benzoxepine-4-carboxamide (1.4 g) and methyl iodide (0.58 ml) in dimethylformamide (50 ml) was stirred at room temperature over night. The solvent was evaporated, and to the residue was added ethyl acetate. Precipitated crude crystal was filtered, which were recrystallized from ethanol-ethyl acetate to give 1—(N-(7—(4-methylphenyl)-2,3-dihydro-1-benzoxepin-4-carbonyl)-4-aminobenzyl)-1-methylpiperidinium iodide (Compound 96) (1.6 g) as colorless crystals.

후처리

  1. customThe solvent was evaporated
  2. additionto the residue was added ethyl acetate
  3. customPrecipitated crude crystal
  4. filtrationwas filtered
  5. customwhich were recrystallized from ethanol-ethyl acetate

출처 및 근거

ORD 기록
ord-5b2ea8ba2f9c4df591173434bef49b76
출처 데이터셋
uspto-grants-2002_07
특허 번호
US06413947B1

반응 노트

불러오는 중…