反应详情

To a solution of the product of Example 146 Step 2 (0.28 g, 1.0 mmol) in 5 mL HOAc was added Cl2 in HOAc (3.0 mL, −1.5 mmol). After 0.75 h, the reaction was treated with Zn dust for 1.5 h. The reaction mixture was decanted from the Zn and concentrated under vacuum. The resulting residue was triturated with H2O, filtered, and washed with H2O. The yield of 6-chloro-7-cyclopropyl-2-(trifluoromethyl)-2H-chromene-3-carboxylic acid was 0.26 g (82%) after drying overnight in a vacuum oven at 50° C.

1. customThe reaction mixture was decanted from the Zn
2. concentrationconcentrated under vacuum
3. customThe resulting residue was triturated with H2O
4. filtrationfiltered
5. washwashed with H2O
6. customafter drying overnight in a vacuum oven at 50° C.