Dichloromethane → Rocuronium Bromide Impurity 31

Participants

Reaction Steps

Acetyl chloride (10.0 ml) was added to a stirred suspension of (2β,3α,5α,16β,17β)-2-(4-morpholinyl)-16-(1pyrrolidinyl)-androstane-3,17-diol (10.0 g) in dichloromethane (100 ml). After 24 h. at room temperature, saturated potassium bicarbonate solution (approx. 20 ml) was added to give pH>7; the dichloromethane layer was separated, washed with water (3×150 ml), dried (Na2SO4) and evaporated to dryness to afford (2β,3α,5α,16β,17β)-2-(4-morpholinyl)-16-(1pyrrolidinyl)-androstane-3,17-diol diacetate as an off-white froth (7.78 g), [α]D20 =+11.4° (c 0.57 in CHCl3)

Provenance & Evidence