Hydrochloric Acid → HCID 21995836, compound

HRID 1978553Notes

Reaction equation

HRID 1978553 reaction equation
[CH2:1]([O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]2[CH:11]=[CH:12][C:13]3[S:19](=[O:21])(=[O:20])[CH2:18][CH2:17][C:16]([C:22]([NH:24][C:25]4[CH:30]=[CH:29][C:28]([CH2:31][N:32]([CH3:39])[CH:33]5[CH2:38][CH2:37][O:36][CH2:35][CH2:34]5)=[CH:27][CH:26]=4)=[O:23])=[CH:15][C:14]=3[CH:40]=2)=[CH:6][CH:5]=1)[CH3:2].[ClH:41]>C1COCC1>[ClH:41].[CH2:1]([O:3][C:4]1[CH:5]=[CH:6][C:7]([C:10]2[CH:11]=[CH:12][C:13]3[S:19](=[O:21])(=[O:20])[CH2:18][CH2:17][C:16]([C:22]([NH:24][C:25]4[CH:30]=[CH:29][C:28]([CH2:31][N:32]([CH3:39])[CH:33]5[CH2:38][CH2:37][O:36][CH2:35][CH2:34]5)=[CH:27][CH:26]=4)=[O:23])=[CH:15][C:14]=3[CH:40]=2)=[CH:8][CH:9]=1)[CH3:2]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 21995680HCID 21995680, compound

Product 1

HCID 21995836HCID 21995836, compound

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent

Procedure

To a solution of 7-(4-ethoxyphenyl)-N-[4-[N-methyl-N-(tetrahydropyran-4-yl)aminomethyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide (2.5 g) in THF (125 ml) was added at room temperature 6N hydrochloric acid (1.5 ml), and the mixture was stirred for 0.5 hour and concentrated under reduced pressure. To the mixture was added diethylether, colorless crystals were collected by filtration to give crude crystals (2.61 g), which were purified with recrystallization from 90% ethanol to give colorless crystals of 7-(4-ethoxyphenyl)-N-[4-[N-methyl-N-(tetrahydropyran-4-yl)aminomethyl]phenyl]-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxamide hydrochloride (Compound 5) (2.33 g).

Workup

  1. concentrationconcentrated under reduced pressure
  2. additionTo the mixture was added diethylether, colorless crystals
  3. filtrationwere collected by filtration
  4. customto give crude crystals (2.61 g), which
  5. customwere purified with recrystallization from 90% ethanol

Sources & evidence

ORD record
ord-63d631190f984ccb9efde15102fd9395
Source dataset
uspto-grants-2001_05
Patent number
US06235771B1

Reaction notes

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