Reaction #1127060
Related Literature (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US07157457B2
Conditions: temp:22.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
Procedure: Intermediate 40 (0.0225 g) and N,N-diisopropylethylamine (0.021 ml) were added to a solution of Intermediate 10 (0.044 g) in dichloromethane (3 ml), and the mixture was shaken at 22° C. for 19 h. Formyl polystyrene scavenging resin (2.95 mmol/g, 0.02 g) was added and the mixture shaken for 2 h. The mixture was filtered, the resin washed with dichloromethane, and the filtrate applied directly to a sulphonic acid ion exchange cartridge (2 g Isolute SCX). Elution with methanol followed by 10% 0.880 ammonia in methanol gave the crude product (0.04 g). Purification by chromatography on silica gel (Varian Bond Elut 1 g cartridge), eluting with dichloromethane, ether, ethyl acetate, and acetone, gave the title compound (0.029 mg). the mixture shaken for 2 h The mixture was filtered the resin washed with dichloromethane Elution with methanol gave the crude product (0.04 g) Purification by chromatography on silica gel (Varian Bond Elut 1 g cartridge) eluting with dichloromethane, ether, ethyl acetate, and acetone
Source ID: ord-e3ac4aed36c247bbbb40385d346c0452