Dichloromethane → HCID 57482543, compound

A solution of 1.22 g (3.7 mmol) of tert-butyl 4-benzo[b]thiophen-4-yl-3-methylpiperazin-1-carboxylate in methylene chloride (12 ml) was added to trifluoroacetic acid (6 ml), and the mixture was stirred at room temperature for 1 hour. The reaction mixture was concentrated under reduced pressure, then an aqueous solution of 5% potassium carbonate was added to the residue and the resulting mixture was extracted with methylene chloride. The organic phase was dried over magnesium sulfate and concentrated under reduced pressure. Concentrated hydrochloric acid (6 ml) and methanol (10 ml) were added to the residue and the resulting mixture was concentrated under reduced pressure. The residue was recrystallized from acetonitrile to obtain 1-benzo[b]thiophen-4-yl-2-methylpiperazine dihydrochloride (0.98 g) as light brown powder.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additionan aqueous solution of 5% potassium carbonate was added to the residue
3. extractionthe resulting mixture was extracted with methylene chloride
4. dry with materialThe organic phase was dried over magnesium sulfate
5. concentrationconcentrated under reduced pressure
6. additionConcentrated hydrochloric acid (6 ml) and methanol (10 ml) were added to the residue
7. concentrationthe resulting mixture was concentrated under reduced pressure
8. customThe residue was recrystallized from acetonitrile

ORD record

ord-8f071284ce694a65847f4912ad0cbbb9

Source dataset

uspto-grants-2015_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09206167B2