Hydrogen chloride-ethyl acetate → N-[1-[(thiazol-4-yl)methyl]piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide Trihydrochloride

HRID 1978459노트

반응식

HRID 1978459 반응식
[S:1]1[CH:5]=[C:4]([CH2:6][N:7]2[CH2:12][CH2:11][CH:10]([CH2:13][NH:14][C:15]([C:17]3[S:27][C:26]4[N:28]5[C:19](=[CH:20][N:21]=[C:22]5[CH:23]=[CH:24][CH:25]=4)[CH:18]=3)=[O:16])[CH2:9][CH2:8]2)[N:3]=[CH:2]1.[ClH:29].C(OCC)(=O)C>C(O)C>[ClH:29].[ClH:29].[ClH:29].[S:1]1[CH:5]=[C:4]([CH2:6][N:7]2[CH2:8][CH2:9][CH:10]([CH2:13][NH:14][C:15]([C:17]3[S:27][C:26]4[N:28]5[C:19](=[CH:20][N:21]=[C:22]5[CH:23]=[CH:24][CH:25]=4)[CH:18]=3)=[O:16])[CH2:11][CH2:12]2)[N:3]=[CH:2]1

참가 물질

4

반응물 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 21993714N-(1-[(thiazol-4-yl)methyl]piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide

생성물 1

HCID 21994197N-[1-[(thiazol-4-yl)methyl]piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide Trihydrochloride수율 28%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

To a solution of N-[1-[(thiazol-4-yl)methyl]piperidin-4-ylmethyl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol was added 2 ml (8.0 mM) of 4N-HCl/ethyl acetate. The solvent was distilled off under reduced pressure and the residue was diluted with ether. The crystals that formed were harvested by filtration and rinsed with ethanol and diethyl ether to provide the title compound as orange-colored crystals (150 mg, 28%).

후처리

  1. distillationThe solvent was distilled off under reduced pressure
  2. additionthe residue was diluted with ether
  3. customThe crystals that formed
  4. filtrationwere harvested by filtration
  5. washrinsed with ethanol and diethyl ether

출처 및 근거

ORD 기록
ord-2ddab0d055624d3a97c86614a726e537
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06235731B1

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