Ethyl Acetate → HCID 131715063, compound

Participants

Reaction Conditions

Reaction Steps

2-Methylthio-11-dimethylaminomethyl-6,11-dihydrodibenz(b,e)oxepin-11-ol, hydrochloride (1.404 g, 4 mmole) is dissolved in 8 ml of trifluoroacetic acid and cooled to -30° C. 8.6 ml of 4M solution of peroxytrifluoro acetic acid in trifluoroacetic acid is added dropwise. The solution is allowed to stay at room temperature. A controlled exothermic reaction starts. After 30 minutes the reaction is complete (the reaction is readily followed by NMR). The solvent is poured into an excess solid sodiumbicarbonate-water mixture and ethyl acetate. The organic extract is washed with 10% sodium bicarbonate and dried over anhydrous sodium sulphate. The desired compound, 2-methylsulfonyl-11-dimethylaminomethyl-6,11-dihydrodibenz(b,e)oxepin-11-ol, hydrochloride, is isolated. M M.p. 247° C. (compound 7:1)

Provenance & Evidence