Chloroform → HCID 18789151, compound

Temperature

100 °C

To 5.36 g (21.35 mmol) of ethyl 6-(2-hydroxyethyl)-pyrazolo-[1,5-a]pyrimidin-7(4H)-one-5-carboxylate were added 7 ml (d=1.645, 75.10 mmol) of phosphorus oxychloride, and the mixture was stirred for 40 minutes in an oil bath heated to 100° C. under a nitrogen atmosphere. The reaction mixture was then cooled to about room temperature, and 7 ml (d=0.726, 50.32 mmol) of triethylamine were added to the mixture. The resultant mixture was stirred for 30 minutes in the oil bath heated to 100° C. Thereafter, the reaction mixture was cooled with ice water, and 100 ml of chloroform were added thereto. The resultant mixture was poured into 600 ml of ice water. The chloroform layer was separated, and the water layer was extracted with chloroform (100 ml×2). After all the chloroform layers were put together and dried over anhydrous magnesium sulfate, the solvent was distilled off. The residue was subjected to column chromatography on silica gel (chloroform) to obtain 3.60 g (yield: 58.5%) of the intended product.

1. temperatureThe reaction mixture was then cooled to about room temperature
2. temperatureheated to 100° C
3. additionwere added
4. customThe chloroform layer was separated
5. extractionthe water layer was extracted with chloroform (100 ml×2)
6. dry with materialdried over anhydrous magnesium sulfate
7. distillationthe solvent was distilled off

ORD record

ord-e523edcf32514694965f0eec01dae5c0

Source dataset

uspto-grants-2000_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06057330