Acetic Acid → 2-(4-Chlorophenyl)-4,5-dimethyl-1,3-oxazol 3-oxide

1.00 g (9.89 mmol) of diacetyl monoxime and 1.53 g (10.88 mmol) of 4-chlorobenzaldehyde were initially charged in 2 ml (34.94 mmol) of glacial acetic acid. Then, while the reaction mixture was cooled with ice, hydrogen chloride gas was introduced for 30 min. 10 ml of diethyl ether were then added to the reaction mixture. A precipitate was formed which was filtered off and washed twice with in each case 2 ml of diethyl ether. The precipitate was resuspended in about 5 ml of water and the suspension was made basic using 25% strength aqueous ammonia solution. The mixture was extracted four times with in each case 10 ml of dichloromethane. The combined organic phases were dried over magnesium sulfate and the solvent was removed on a rotary evaporator. Without further purification, the residue was used for the next reaction.

1. additionwas introduced for 30 min
2. customA precipitate was formed which
3. filtrationwas filtered off
4. washwashed twice with in each case 2 ml of diethyl ether
5. extractionThe mixture was extracted four times with in each case 10 ml of dichloromethane
6. dry with materialThe combined organic phases were dried over magnesium sulfate
7. customthe solvent was removed on a rotary evaporator
8. customWithout further purification
9. customthe residue was used for the next reaction

ORDレコード

ord-c5115581a6af491e8b88c977cca06d60

出典データセット

uspto-grants-2013_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08618119B2