反应详情

温度

80 °C

The product from step 1(200 mg, 1.0 mmoles) and thio phenol (110 mg, 1 mmoles) were combined in dimethyl formamide (1.5 mL) at room temperature. Lithium (bis trimethyl silyl) amide (1.25 mL of a 1M solution in THF) was added and the reaction heated at 80° C. for 18 h. Reaction was diluted with water, made acidic with acetic acid and extracted with dichloromethane 2×40 mL. The combined extracts were washed with water 2×50 mL, brine 1×50 mL, dried and the solvent removed under pressure. The crude was chromatographed to give the product 108 mg (35%). MS (ESI+) for C16H22O4S m/z 333 (M+Na)+.

1. customReaction
2. extractionextracted with dichloromethane 2×40 mL
3. washThe combined extracts were washed with water 2×50 mL, brine 1×50 mL
4. customdried
5. customthe solvent removed under pressure
6. customThe crude was chromatographed