1,4-Dioxane → 3-{2-[4-(2,6-Dichloro-benzyloxy)-phenyl]-morpholin-4-yl}-propionic acid hydrochloride

3-{2-[4-(2,6-Dichloro-benzyloxy)-phenyl]-morpholin-4-yl}-propionic acid. 3-{2-[4-(2,6-Dichloro-benzyloxy)-phenyl]-morpholin-4-yl}-propionic acid tert-butyl ester (0.59 g; 1.27 mmol) was dissolved in a 4M solution of HCl in 1,4-dioxane (6.33 mL, 25.30 mmol) and stirred overnight at RT. Subsequently, the solvent was removed in vacuo and the residue treated with iPr2O, the precipitate was collected by filtration and dried overnight under reduced pressure to afford 3-{2-[4-(2,6-Dichloro-benzyloxy)-phenyl]-morpholin-4-yl}-propionic acid hydrochloride (0.50 g). 1H NMR (400 MHz, DMSO-d6) δ ppm 2.88-2.97 (2H, m) 3.11 (1H, t, J=11.7 Hz) 3.15-3.23 (1H, m) 3.30-3.43 (2H, m) 3.49 (1H, d, J=12.0 Hz) 3.55-3.64 (1H, m) 4.01-4.20 (2H, m) 4.88 (1H, d, J=12.0 Hz) 5.24 (2H, s) 7.04-7.12 (2H, m) 7.35 (2H, d, J=8.7 Hz) 7.40-7.49 (1H, m) 7.49-7.56 (2H, m).

1. customSubsequently, the solvent was removed in vacuo
2. additionthe residue treated with iPr2O
3. filtrationthe precipitate was collected by filtration
4. customdried overnight under reduced pressure

ORDレコード

ord-be555cf6d1db4d21956eb41ca4b224ab

出典データセット

uspto-grants-2015_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09045441B2