3-Chloro-1,2-propanediol → 2,3-Dihydroxypropyl-3-aminobenzotrifluoride

In a two liter three necked flask equipped with mechanical stirrer, refluxing condenser and thermometer was added 322.2 gms (2.0 moles) of 3-aminobenzotrifluoride, 500 ml of ethoxyethanol solvent and 442.0 gms (4 moles) 1-chloro-2,3-propanediol. While this mixture was cooling, 205 gms (2.36 moles) of sodium carbonate was added keeping the temperature below 35° C. The mixture was then heated to reflux for 24 hours. Afterwards, the crude reaction mixture was filtered from the salt by-product. The salt was then washed several times with chloroform and these washings were combined with the filtrate. The solvent and chloroform was then removed under low vacuum and high vacuum to give 450.5 gms of the crude bis-2,3-dihydroxypropyl-3-aminobenzotrifluoride as a viscous dark oil.

1. temperaturerefluxing condenser
2. temperatureWhile this mixture was cooling
3. customthe temperature below 35° C
4. temperatureThe mixture was then heated
5. temperatureto reflux for 24 hours
6. customAfterwards, the crude reaction mixture
7. filtrationwas filtered from the salt by-product
8. washThe salt was then washed several times with chloroform
9. customThe solvent and chloroform was then removed under low vacuum and high vacuum

ORDレコード

ord-c708e6e536f34a48971a856e4648a83a

出典データセット

uspto-grants-1988_08

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04761502