Acetic Anhydride → HCID 10465110, Verbindung

Temperatur

0 °C

A suspension of 2,3,4,5-tetrahydro-1H-2-benzazepine hydrochloride (10 g, 54.4 mmol) in dry dichloromethane (450 mL) was stirred at 0° C. Triethylamine (18.21 mL, 130.6 mmol) was added followed by the dropwise addition of acetic anhydride (6.18 mL, 65.3 mmol) in dry dichloromethane (50 mL). The reaction was then stirred for 1 hour whilst allowing the temperature to rise slowly to room temperature. The resulting mixture was washed with 1 N hydrochloric acid (200 mL) and brine (200 mL), dried over sodium sulfate and concentrated in vacuo to give 10 g of product as colorless oil (yield was 97%). It was used in next step without further purification. MS obsd. (ESI+) [(M+H)+] 190.

1. stirringThe reaction was then stirred for 1 hour
2. customto rise slowly to room temperature
3. washThe resulting mixture was washed with 1 N hydrochloric acid (200 mL) and brine (200 mL)
4. dry with materialdried over sodium sulfate
5. concentrationconcentrated in vacuo

ORD-Eintrag

ord-d7039474f4904535a7ee7aefd65b3471

Quelldatensatz

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08871756B2