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

HRID 1978459ノート

反応式

HRID 1978459 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-2ddab0d055624d3a97c86614a726e537
出典データセット
uspto-grants-2001_05
特許番号
US06235731B1

反応ノート

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