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

HRID 1978526노트

반응식

HRID 1978526 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-ddd33cfa13f24474b2138a130c78f5e8
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06235731B1

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