Water → HCID 54215524, compound

Participants

Reaction Steps

Under nitrogen, a solution of title product of Example C1 (0.468 g, 1.59 mmoles) in 5 ml CH2Cl2 was cooled to -78°. Boron tribromide (0.45 ml, 4.77 mmoles) was added. After stirring 20 minutes at ×78°the reaction mixture was allowed to warm to room temperature, stirred 2 hours, diluted with 25 ml. of water and then 20 ml CH2Cl2, stirred 15 minutes, and the pH adjusted to 6-7 with saturated NaHCO3. The aqueous layer was separated and extracted 2×25 ml CH2Cl2. The three organic layers were combined, dried over MgSO4, and concentrated to solids in vacuo, 0.402 g. Recrystallization from CH2Cl2 /hexane gave purified title product, 0.320 g, m.p. 200°-203°.

Provenance & Evidence