反応 #162769

反応方程式

2,2,2-Trichloroethyl chloroformate

Intermediate 12c

5-tert-Butyl-2-[3-(4,4-difluoro-piperidin-1-ylmethyl)-phenyl]-2H-pyrazol-3-ylamine

DIPEA

→

title compound

収率 72.0%

{5-tert-Butyl-2-[3-(4,4-difluoro-piperidin-1-ylmethyl)-phenyl]-2H-pyrazol-3-yl}-carbamic acid 2,2,2-trichloro-ethyl ester

収率 72.0%

溶媒

THF

反応条件

後処理

1. 1
   その他The mixture was then partitioned between water (10 mL) and EtOAc (3×15 mL)
2. 2
   乾燥the combined organic extracts dried (Na2SO4)
3. 3
   その他The solvent was evaporated
4. 4
   その他the residue triturated under pentane
5. 5
   ろ過filtered

実験手順

2,2,2-Trichloroethyl chloroformate (0.077 mL, 0.57 mmol) was added to a solution of Intermediate 12c (200 mg, 0.57 mmol) and DIPEA (0.31 mL, 1.81 mmol) in THF (5 mL), and the mixture stirred for 3 h. The mixture was then partitioned between water (10 mL) and EtOAc (3×15 mL), and the combined organic extracts dried (Na2SO4). The solvent was evaporated and the residue triturated under pentane and filtered to give the title compound as a yellow solid (215 mg, 72%). LCMS (Method 1): Rt 2.89 min, m/z 523/525 [MH+]

出典