反应详情

温度

10 °C

A mixture of EXAMPLE 1 (41.05 Kg) and ammonium formate (5 equivalents), with or without 2,6-di-tert-butylphenol antioxidant, was treated with a mixture of 50% wet 5% palladium hydroxide on carbon (7% by weight per weight of EXAMPLE 1), in DMF (6 mL/g catalyst) then DMF (total DMF volume: 5 mL/g EXAMPLE 1) first with moderate agitation to control an exotherm (typically peaking at 85° C.) then with increased agitation for 1 hour (incomplete reactions were treated with additional catalyst/DMF mixture), cooled to 10° C., and filtered. The filtrant was washed with DMF (0.4 mL/g EXAMPLE 1), and the filtrate was added to water (29.4 mL/g EXAMPLE 1) at 10° C. to precipitate a solid which was filtered, washed with water (7.5 mL/g EXAMPLE 1), partially dried under a nitrogen stream, and further dried under vacuum at 50° C. to about 0.5% moisture.

1. customtypically peaking at 85° C.
2. temperaturewith increased agitation for 1 hour
3. filtrationfiltered
4. washThe filtrant was washed with DMF (0.4 mL/g EXAMPLE 1)
5. additionthe filtrate was added to water (29.4 mL/g EXAMPLE 1) at 10° C.
6. customto precipitate a solid which
7. filtrationwas filtered
8. washwashed with water (7.5 mL/g EXAMPLE 1)
9. custompartially dried under a nitrogen stream
10. customfurther dried under vacuum at 50° C. to about 0.5% moisture