Water → HCID 22460334, compound

Participants

Reaction Steps

In 100 g of THF was dissolved 8.8 g (0.038 mol) of the bis (4-hydroxyphenylthio )methane crude product in Synthesis Example 1. 11.5 g (0.11 mol) of triethylamine was added to the solution, which was stirred under ice cooling. 8.9 g (0.11 mol) of acetyl chloride was added dropwise to the solution, which was ripened for one hour in an oil bath at 70° C. After cooling, 26 g of water was added to the solution, which separated into aqueous and organic layers. The organic layer was combined with 100 g of dichloromethane, washed with 100 g of water, and concentrated in vacuum. There was yielded 13 g of an oily residue, which was used in the subsequent reaction without further purification. It is noted that this oily matter crystallized when kept at room temperature.

Provenance & Evidence