Diisopropylethylamine → tert-Butyl 4,4,4-trifluoro-1-oxo-1-(2-(phenylcarbamoyl)-1H-pyrrol-1-ylamino)butan-2-ylcarbamate

421 mg (1.64 mmol) of 2-(tert-butoxycarbonylamino)-4,4,4-trifluorobutanoic acid were suspended in a mixture of N,N-dimethylformamide (5 mL) and dichloromethane (5 mL) and HATU (624 mg, 1.64 mmol) and DIEA (286 μl, 1.64 mmol) were added. The resulting suspension was stirred at room temperature for 2 hours and then 1-amino-N-phenyl-1H-pyrrole-2-carboxamide (300 mg, 1.49 mmol) was added. The resulting solution was stirred at room temperature overnight and the dichloromethane was removed in vacuum. 25 mL of water were added to the remaining solution and, after vigorous stirring, the solid that formed was filtered and washed with water. 582 mg (89% yield) of the title compound were obtained as a white solid.

1. additionwere added
2. stirringThe resulting solution was stirred at room temperature overnight
3. customthe dichloromethane was removed in vacuum
4. addition25 mL of water were added to the remaining solution
5. customafter vigorous stirring, the solid that formed
6. filtrationwas filtered
7. washwashed with water

ORDレコード

ord-a38dff65ca9e494eb2d74d0aa6b7803f

出典データセット

uspto-grants-2016_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US09340547B2