Chloroform → HCID 14698770, compound

To a chloroform solution containing 68.12 g (0.7 mole) of phosgene at 0°-10° C. was added 80 g (0.7 mole) of 1,2-dimethyl-3-pyrrolidinol at a rate to maintain the temperature below 10° C. The reaction mixture was allowed to stir at room temperature overnight. The mixture was cooled in an ice bath and 100 ml of triethylamine was added dropwise maintaining the temperature below 10° C. The mixture was extracted in order with water, 3N hydrochloric acid solution, 3N sodium hydroxide solution and again with water. The chloroform layer was dried over anhydrous sodium sulfate and evaporated to yield 110 g of dark amber oil which was distilled at 113°-118° C. at 0.05 mm to give 80 g (64.8%) of pale yellow oil, n22 =1.4796.

1. temperatureto maintain the temperature below 10° C
2. temperatureThe mixture was cooled in an ice bath
3. temperaturemaintaining the temperature below 10° C
4. extractionThe mixture was extracted in order with water, 3N hydrochloric acid solution, 3N sodium hydroxide solution and again with water
5. dry with materialThe chloroform layer was dried over anhydrous sodium sulfate
6. customevaporated

ORD record

ord-8f5214ffff694f2495e983ca35bb51b0

Source dataset

uspto-grants-1989_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04886794