Diisopropylethylamine → N-{[(2S)-4-(3,4-Dichlorobenzyl)morpholin-2-yl]methyl}N'-[3-(ethylsulfonyl)propyl]urea

温度

22 °C

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).

1. stirringthe mixture shaken for 2 h
2. filtrationThe mixture was filtered
3. washthe resin washed with dichloromethane
4. washElution with methanol
5. customgave the crude product (0.04 g)
6. customPurification by chromatography on silica gel (Varian Bond Elut 1 g cartridge)
7. washeluting with dichloromethane, ether, ethyl acetate, and acetone

ORDレコード

ord-e3ac4aed36c247bbbb40385d346c0452

出典データセット

uspto-grants-2007_01

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US07157457B2