Diisopropylethylamine → HCID 86603093, 화합물

To a solution of 103 mg (0.53 mmol) of 5-chloro-1H-indole-7-carboxylic acid and 169 mg of TBTU (0.53 mmol) in 6 ml DMF, were added 0.45 ml (2.63 mmol) of N,N-diisopropylethyl amine. After stirring for 5 min at rt, 200 mg (0.57 mmol) of (4-tert-butyl-benzyl)-[2-(3-fluoro-5-trifluoromethyl-phenyl)-ethyl]-amine in 2 ml DMF were added. After stirring for 3 h at rt, the reaction mixture was diluted with 80 ml water and extracted with EtOAc (2×). The combined organic phases were washed with water and brine, dried with magnesium sulfate, filtered and concentrated in vacuo. The residue was purified by column chromatography (40 g silica gel; DCM/heptane 9:1) to give 211 mg white solid (70%). MS (EI) 530.2 (M)+.

1. stirringAfter stirring for 3 h at rt
2. extractionextracted with EtOAc (2×)
3. washThe combined organic phases were washed with water and brine
4. dry with materialdried with magnesium sulfate
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was purified by column chromatography (40 g silica gel; DCM/heptane 9:1)

ORD 기록

ord-c362b241839f4850a47eaadbdf6bd320

출처 데이터셋

uspto-grants-2007_08

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US07259183B2