Formic Acid → HCID 21088387、化合物

温度

60 °C

12.6 ml of formic acid were added dropwise at 0° C. to 15 ml of acetic anhydride, and the mixture was then stirred for 2 hours at 60° C. After cooling to 20° C., the mixture was diluted with 140 ml of tetrahydrofuran, cooled to −4° C., and at this temperature a solution of 18.4 g of 2-(2-aminophenyl)ethanol in 185 ml of tetrahydrofuran was added dropwise. After stirring for 3 hours at −6° C. the mixture was neutralised with aqueous potassium hydrogen carbonate solution (25% KHCO3) and extracted four times with 300 ml of ethyl acetate each time. The combined extracts were dried over sodium sulfate and concentrated by evaporation in vacuo. 18.4 g (94% of theory) of the title compound were thereby obtained in the form of yellowish crystals that melted at 49–54° C.

1. temperatureAfter cooling to 20° C.
2. temperaturecooled to −4° C.
3. stirringAfter stirring for 3 hours at −6° C. the mixture
4. extractionextracted four times with 300 ml of ethyl acetate each time
5. dry with materialThe combined extracts were dried over sodium sulfate
6. concentrationconcentrated by evaporation in vacuo

ORDレコード

ord-51ee964ad2ee4f0bb2b2ff761a5b33c9

出典データセット

uspto-grants-2007_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07183274B2