Sulfuric Acid → 1-(3-Bromo-8-chloro-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridin-11-yl)-4-[(4-piperidinyl)acetyl]piperazine

関与物質

役割	名称	HCID	仕込み量
反応物	Sulfuric Acid	HCID 1118	—
反応物	Sodium Hydroxide	HCID 14798	—
反応物	1,1-Dimethylethyl 4-[[[4-(3-bromo-8-chloro-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridin-11-YL)-1-piperazinyl]carbonyl]methyl]-1-piperidinecarboxylate	HCID 10841523	—
溶媒	Methanol	HCID 887	—
溶媒	1,4-Dioxane	HCID 31275	—
生成物	1-(3-Bromo-8-chloro-6,11-dihydro-5H-benzo[5,6]cyclohepta[1,2-b]pyridin-11-yl)-4-[(4-piperidinyl)acetyl]piperazine	HCID 10768220	74%

反応条件

温度	25 °C

反応手順

The title compound from Step A above (4.61 g) (7.5 mmoles) was dissolved in methanol (40 mL) and a 10% (v/v) conc. H2SO4 in dioxane solution (100 mL) was added. The mixture was stirred at 25° C. for 2 h and then basified with conc. aqueous NaOH. The mixture was extracted with dichloromethane and the latter was washed with water, dried over MgSO4, filtered and evaporated to dryness. The product was chromatographed on silica gel using 10% (10% conc. NH4OH in methanol)dichloromethane as the eluant to give the title compound (Yield: 2.86 g; 74%)

情報源と証拠

DOI	10.6084/m9.figshare.5104873.v1
特許番号	US06699872B2
出典データセット	uspto-grants-2004_03
ORD ID	ord-67a6fcbfdb864a4fb2c6c88de14936c7
出典メモ	uspto-grants-2004_03