Ethyl bromoacetate → 8-Chloro-6-phenyl-2H,4H-pyrrolo[3,4-d][2]benzazepine-2-acetic acid ethyl ester

To a solution of 1.4 g (12.4 mmole) of potassium t-butoxide in 30 ml of dry dimethylformamide was added 2.4 g (8.2 mmole) of 8-chloro-6-phenyl-2H,4H-pyrrolo[3,4-d][2]benzazepine. The mixture was cooled to 0°, and stirred for 10 min. To the mixture was added 1.3 mol (11.7 mmole) of ethyl bromoacetate. The mixture was stirred at 0° for 45 min, diluted with water, and extracted with ether. The ether solution was washed with water, dried with sodium sulfate, and concentrated at reduced pressure to give a yellow oil. Purification by column chromatography (70 g SiO2, 9:1 methylene chloride/ethyl) gave as the first major component a yellow oil.

1. temperatureThe mixture was cooled to 0°
2. stirringThe mixture was stirred at 0° for 45 min
3. extractionextracted with ether
4. washThe ether solution was washed with water
5. dry with materialdried with sodium sulfate
6. concentrationconcentrated at reduced pressure
7. customto give a yellow oil
8. customPurification by column chromatography (70 g SiO2, 9:1 methylene chloride/ethyl)
9. customgave as the first major component a yellow oil

ORDレコード

ord-44b1ce954f2c4a90b022c4e43976b842

出典データセット

uspto-grants-1984_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04431823