Triethylamine → HCID 86585984, compound

Participants

Reaction Steps

The alcohol prepared in Step 5 (11.3 g, 26.6 mmol) is dissolved in CH2Cl2 (125 ml) with triethylamine (11.0 ml, 79 mmol) and cooled to 0°. Methanesulfonylchloride (2.4 ml, 31 mmol) is added and the reaction stirred for 2 hours. Extra CH2Cl2 (100 ml) is added and the solution washed with water (100 ml) and brine (50 ml) then dried (MgSO4). Evaporation gave a gum which is chromatographed over silica gel (500 g) eluting with 25-60% ethyl acetate-hexane. The product is obtained as a white foam (10.95 g, 82%): HRMS (FAB): Calcd for m+Na=525.1672; Found: 525.1671. Anal: Calcd. for C25H30N2O7S: C, 59.74; H, 6.02; N, 5.57. Found: C, 59.44; H, 6.07; N, 5.49.

Provenance & Evidence