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 1978552Notes

Reaction equation

HRID 1978552 reaction equation
[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

Participants

4

Reactant 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

Product 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

Reagents, catalysts & solvents 1

HCID 18681192Ethanol, mixt. with methanolSolvent

Procedure

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).

Workup

  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

Sources & evidence

ORD record
ord-7a05e466162d495ea2c3760fda62e9b4
Source dataset
uspto-grants-2001_05
Patent number
US06235771B1

Reaction notes

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