Ammonium Chloride → (S)-N-(3-(3-(2-Amino-4-chloro-5-(2-(methoxymethyl)pyrrolidin-1-yl)phenyl)thioureido)-4-chlorobenzyl)-1-(trifluoromethyl)cyclopropanecarboxamide

온도

90 °C

A mixture of (S)—N-(4-chloro-3-(3-(4-chloro-5-(2-(methoxymethyl)pyrrolidin-1-yl)-2-nitrophenyl)thioureido)benzyl)-1-(trifluoromethyl)cyclopropanecarboxamide (145 mg; 0.23 mmol), Fe (65 mg; 1.2 mmol), saturated aqueous NH4Cl-solution (3 mL) and EtOH (3 mL) was stirred at 90° C. for 2 h. The mixture was basicified to pH-9-10 and filtered through celite. The celite pad was washed with EtOH and EtOAc. The mixture was concentrated and the residue was extracted with EtOAc. The organic layer was dried over Na2SO4, filtered and concentrated. The residue was washed with Et2O to give the sub-title compound.

1. filtrationfiltered through celite
2. washThe celite pad was washed with EtOH and EtOAc
3. concentrationThe mixture was concentrated
4. extractionthe residue was extracted with EtOAc
5. dry with materialThe organic layer was dried over Na2SO4
6. filtrationfiltered
7. concentrationconcentrated
8. washThe residue was washed with Et2O

ORD 기록

ord-319a60ff269c4968a7a269ed776812f6

출처 데이터셋

uspto-grants-2013_06

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08466186B2