Isobutyric Acid → HCID 19936152、化合物
反応式
Br[C:2](Cl)([C:9]([F:12])([F:11])[F:10])[CH:3](O)[CH:4]=[C:5]([CH3:7])[CH3:6].C(OC)(OC)(OC)C.C(O)(=O)C(C)C>>[CH3:6][C:5](=[CH:4][CH2:3][CH2:2][C:9]([F:12])([F:11])[F:10])[CH3:7]参加物
4
反応条件
- 温度
- 111 °C
実験手順
5-Bromo-5-chloro-4-hydroxy-2-methyl-6,6,6-trifluorohex-2ene (10.0 g), trimethyl orthoacetate (48.0 g) and isobutyric acid (0.29 g) were charged to a round-bottomed flask fitted with: nitrogen inlet/bubbler, thermometer and Dean and Stark received packed with 5A molecular seives. The mixture was heated with agitation to reflux and distillates collected until reaction mass temperature increased to 111° C. (ca. 1 hr). Once the reaction was complete, the residual trimethyl orthoacetate was removed by distillation under vacuum (ca. 50° C. ≃50 mmHg) to give the product, 5-bromo-5-chloro-4-1,1-dimethoxyethoxy)-2-methyl-6,6,6-trifluorohex-2-ene, as an orange oil (10.9 g, 85% yield).