Hydrochloric Acid → N-[1-[3-(2-methoxycarbonylphenoxy)propan-1-yl]piperidin-4-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide dihydrochloride

HRID 1978526ノート

反応式

HRID 1978526 の反応式
[CH3:1][O:2][C:3]([C:5]1[CH:35]=[CH:34][CH:33]=[CH:32][C:6]=1[O:7][CH2:8][CH2:9][CH2:10][N:11]1[CH2:16][CH2:15][CH:14]([NH:17][C:18]([C:20]2[S:30][C:29]3[N:31]4[C:22](=[CH:23][N:24]=[C:25]4[CH:26]=[CH:27][CH:28]=3)[CH:21]=2)=[O:19])[CH2:13][CH2:12]1)=[O:4].[ClH:36]>C(O)C>[ClH:36].[ClH:36].[CH3:1][O:2][C:3]([C:5]1[CH:35]=[CH:34][CH:33]=[CH:32][C:6]=1[O:7][CH2:8][CH2:9][CH2:10][N:11]1[CH2:16][CH2:15][CH:14]([NH:17][C:18]([C:20]2[S:30][C:29]3[N:31]4[C:22](=[CH:23][N:24]=[C:25]4[CH:26]=[CH:27][CH:28]=3)[CH:21]=2)=[O:19])[CH2:13][CH2:12]1)=[O:4]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 21993853N-[1-[3-(2-methoxycarbonylphenoxy)propan-1-yl]piperidin-4-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide

生成物 1

HCID 21994086N-[1-[3-(2-methoxycarbonylphenoxy)propan-1-yl]piperidin-4-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide dihydrochloride収率 87%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

To a solution of 0.81 g (1.64 inmol.) of N-[1-[3-(2-methoxycarbonylphenoxy)propan-1-yl]piperidin-4-yl]-5-thia-1,8b-diazaacenaphthylene-4-carboxamide in ethanol (5 ml) was added, at room temperature, 1 ml (12 mmol.) of 12N hydrochloric acid. The mixture was stirred for several minutes. The reaction mixture was concentrated, to which was added acetonitrile. The resulting crystalline precipitate was collected by filtration, which was washed with ethanol and diethyl ether to give the object compound (809.1 mg, 87%) as orange crystals, m.p.164-168° C.

後処理

  1. concentrationThe reaction mixture was concentrated, to which
  2. additionwas added acetonitrile
  3. filtrationThe resulting crystalline precipitate was collected by filtration, which
  4. washwas washed with ethanol and diethyl ether

出典と根拠

ORDレコード
ord-ddd33cfa13f24474b2138a130c78f5e8
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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