Reaktion #71684

Reaktionsgleichung

H2O

HBTU

DIPEA

(3R)-3-methyl-1-{[4-(trifluoromethyl)phenyl]sulfonyl}piperazine

2-methyl-3-pyridinecarboxylic acid

HOBT

→

title compound

Ausbeute 122.3%

(2R)-2-methyl-1-[(2-methyl-3-pyridinyl)carbonyl]-4-{[4-(trifluoromethyl)phenyl]sulfonyl}piperazine formic acid salt

Ausbeute 122.3%

Lösungsmittel

DMF

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe DMF was evaporated under vacuum, 5 ml of DCM
2. 2
   workup.ADDITIONadded
3. 3
   Waschenwashed with saturated NaHCO3 solution (5 ml)
4. 4
   Sonstigedried on a phase separation cartridge
5. 5
   Sonstigeevaporated under vacuo
6. 6
   workup.DISSOLUTIONThe crude material was dissolved in MeCN/DMSO 1:1
7. 7
   Sonstigepurified by MDAP

Vorschrift

To a solution of (3R)-3-methyl-1-{[4-(trifluoromethyl)phenyl]sulfonyl}piperazine (Description 12) (80 mg, 0.259 mmol) in DMF (4 ml) was added 2-methyl-3-pyridinecarboxylic acid (35.6 mg, 0.259 mmol), HOBT.H2O (39.7 mg, 0.259 mmol), HBTU (98 mg, 0.259 mmol) and DIPEA (0.136 ml, 0.778 mmol) and the reaction mixture was stirred at room temperature for 1 h. The DMF was evaporated under vacuum, 5 ml of DCM added and then washed with saturated NaHCO3 solution (5 ml), dried on a phase separation cartridge and evaporated under vacuo. The crude material was dissolved in MeCN/DMSO 1:1 and purified by MDAP to give the title compound (75 mg).

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