反应详情

温度

32.5 °C

3,4-dichloroaniline (150 g) in TBME (1L) was cooled to 10-15° C. 30% aq NaOH (141 g, 1.14 equiv) was added, and the solution stirred vigorously via overhead mechanical stirrer. Trimethylacetyl chloride (“PivCl”, 126 mL) was added at such a rate as to keep the internal temperature below 30° C. During this addition, the solution mixture becomes thick with white solid product. When the addition was complete (10-15 min), the mixture was heated to 30-35° C. for 1 hr, and then allowed to cool. The reaction mixture was held at −5° C. (overnight), and then filtered, rinsing first with 90:10 water/MeOH (600 mL) and then water (900 mL). Drying under vacuum yielded 195 g (86%) product, as off-white crystals. LCMS m/z 246(M−H)+.

1. customthe internal temperature below 30° C
2. additionDuring this addition
3. additionWhen the addition
4. custom(10-15 min)
5. temperatureto cool
6. customwas held at −5° C.
7. custom(overnight)
8. filtrationfiltered
9. washrinsing first with 90:10 water/MeOH (600 mL)
10. customDrying under vacuum