Dichloromethane → HCID 67345859、化合物

反応式

[S:1](N)([NH2:4])(=[O:3])=[O:2].[CH:6]1([CH2:9][NH:10][CH2:11][CH:12]([O:15][CH3:16])[O:13][CH3:14])[CH2:8][CH2:7]1.C(Cl)Cl>O1CCOCC1>[CH:6]1([CH2:9][N:10]([CH2:11][CH:12]([O:13][CH3:14])[O:15][CH3:16])[S:1]([NH2:4])(=[O:3])=[O:2])[CH2:7][CH2:8]1

参加物

実験手順

Sulfamide (5 eq) was added to a solution of N-(cyclopropylmethyl)-(2,2-dimethoxyethanamine) in dioxane (0.12 M). The reaction was stirred at reflux overnight. The solvent was removed in vacuo, the residue taken up in EtOAc and washed with H2O, brine, before being dried (Na2SO4), filtered and concentrated in vacuo to give the crude material. DCM was added and the resultant precipitate removed by filtration, while the filtrate was concentrated in vacuo to afford the product (68%). 1H NMR (300 MHz, DMSO-d6, 300 K) δ 0.15-0.19 (m, 2H), 0.44-0.47 (m, 2H), 1.03-1.05 (m, 1H), 2.95-2.98 (m, 2H), 3.17-3.19 (m, 2H), 3.28 (s, 6H), 4.51 (t, J 5.0, 1H), 6.63 (s, 2H).