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Hydrochloric Acid → N-[4-[N-methyl-N-(tetrahydropyran-4-yl)aminomethyl]phenyl]-7-(4-morpholinophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide dihydrochloride

HRID 1978552
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HRID 1978552 반응식
[CH3:1][N:2]([CH2:9][C:10]1[CH:15]=[CH:14][C:13]([NH:16][C:17]([C:19]2[CH2:20][CH2:21][S:22](=[O:43])(=[O:42])[C:23]3[CH:29]=[CH:28][C:27]([C:30]4[CH:35]=[CH:34][C:33]([N:36]5[CH2:41][CH2:40][O:39][CH2:38][CH2:37]5)=[CH:32][CH:31]=4)=[CH:26][C:24]=3[CH:25]=2)=[O:18])=[CH:12][CH:11]=1)[CH:3]1[CH2:8][CH2:7][O:6][CH2:5][CH2:4]1.[ClH:44]>C(O)C.CO>[ClH:44].[ClH:44].[CH3:1][N:2]([CH2:9][C:10]1[CH:15]=[CH:14][C:13]([NH:16][C:17]([C:19]2[CH2:20][CH2:21][S:22](=[O:43])(=[O:42])[C:23]3[CH:29]=[CH:28][C:27]([C:30]4[CH:35]=[CH:34][C:33]([N:36]5[CH2:41][CH2:40][O:39][CH2:38][CH2:37]5)=[CH:32][CH:31]=4)=[CH:26][C:24]=3[CH:25]=2)=[O:18])=[CH:12][CH:11]=1)[CH:3]1[CH2:8][CH2:7][O:6][CH2:5][CH2:4]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 3009393N-[4-[[methyl(tetrahydropyran-4-yl)amino]methyl]phenyl]-7-(4-morpholinophenyl)-1,1-dioxo-2,3-dihydro-1$l^{6}-benzothiepine-4-carboxamide

생성물 1

HCID 21995875N-[4-[N-methyl-N-(tetrahydropyran-4-yl)aminomethyl]phenyl]-7-(4-morpholinophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide dihydrochloride

시약·촉매·용매 1

HCID 18681192Ethanol, mixt. with methanol용매

실험 절차

To a solution of N-[4-[N-methyl-N-(tetrahydropyran-4-yl)aminomethyl]phenyl]-7-(4-morpholinophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (36 mg) in ethanol/methanol (10/5 ml) was added at room temperature concentrated hydrochloric acid (0.5 ml), and the mixture was stirred for a few minutes. Insoluble materials were filtered off, and the filtrate was concentrated under reduced pressure. To the residue was added diethylether, and precipitated solid was collected by filtration, which was washed with diethylether to give yellow powder of N-[4-[N-methyl-N-(tetrahydropyran-4-yl)aminomethyl]phenyl]-7-(4-morpholinophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide dihydrochloride (Compound 2) (34 mg).

후처리

  1. filtrationInsoluble materials were filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionTo the residue was added diethylether
  4. customprecipitated solid
  5. filtrationwas collected by filtration, which
  6. washwas washed with diethylether

출처 및 근거

ORD 기록
ord-7a05e466162d495ea2c3760fda62e9b4
출처 데이터셋
uspto-grants-2001_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06235771B1

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