Triethylamine → (R)-benzyl 4-(dimethylamino)-3-(5-(1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-yl)thiophene-2-sulfonamido)butanoate

To a solution of (R)-benzyl 3-amino-4-(dimethylamino)butanoate (27 mg, 0.086 mmol), triethylamine (50 μL, 0.36 mmol) and DMAP (1 mg, 0.008 mmol) in anhydrous CH2Cl2 (1 mL) was added 5-(1-methyl-3-(trifluoromethyl)-1H-pyrazol-5-yl)thiophene-2-sulfonyl chloride (82 mg, 0.25 mmol). The solution was stirred overnight at room temperature. The solvents were removed in vacuo and the residue was purified by preparatory HPLC. The residue was dissolved into CH2Cl2 (50 mL) and washed with 0.1 N NaOH (5 mL), dried over MgSO4 and concentrated to give the title compound as a white solid (26 mg, 57%). MS ESI 531.2 [M+H]+, calcd for [C22H25F3N4O4S2+H]+ 531.13.

1. customThe solvents were removed in vacuo
2. customthe residue was purified by preparatory HPLC
3. dissolutionThe residue was dissolved into CH2Cl2 (50 mL)
4. washwashed with 0.1 N NaOH (5 mL)
5. dry with materialdried over MgSO4
6. concentrationconcentrated

ORDレコード

ord-ae4b3133b406488c9935adbbcc96f5e4

出典データセット

uspto-grants-2013_04

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08410150B2