반응 #162793

반응 방정식

2,2,2-trichloroethylchloroformate

Intermediate 24b

5-tert-butyl-2-[2-(2-morpholin-4-yl-ethyl)-2H-indazol-6-yl]-2H-pyrazol-3-ylamine

DIPEA

→

title compound

수율 26.0%

{5-tert-Butyl-2-[2-(2-morpholin-4-yl-ethyl)-2H-indazol-6-yl]-2H-pyrazol-3-yl}-carbamic acid 2,2,2-trichloro-ethyl ester

수율 26.0%

용매

THF

THF

반응 조건

후처리

1. 1
   기타partitioned between EtOAc/water
2. 2
   추출extracted with EtOAc
3. 3
   건조The combined organics were dried over Na2SO4
4. 4
   여과filtered
5. 5
   농축concentrated in vacuo
6. 6
   기타Purification by FCC

실험 절차

To a solution of Intermediate 24b (86 mg, 0.23 mmol) in THF (10 mL) was added DIPEA (80 μL, 0.46 mmol), followed by the dropwise addition of a solution of 2,2,2-trichloroethylchloroformate (32 μL, 0.23 mmol) in THF (2 mL). The mixture was stirred at RT for 4 h, then partitioned between EtOAc/water and extracted with EtOAc. The combined organics were dried over Na2SO4, filtered and concentrated in vacuo. Purification by FCC, using 0-20% MeOH in EtOAc, gave the title compound (32 mg, 26%) as a yellow solid. LCMS (Method 4): Rt 2.64, 0.2 m/z 543, 545 [MH+].

출처