반응 #6982

반응 방정식

5-{[2-(6-bromo-pyridin-2-ylamino)-thiazol-5-ylmethyl]-amino}-N-cyclopropyl-2,4-difluoro-benzamide

N-methyl piperazine

→

title compound

수율 55.0%

N-Cyclopropyl-2,4-difluoro-5-({2-[6-(4-methyl-piperazin-1-yl)-pyridin-2-ylamino]-thiazol-5-ylmethyl}-amino)-benzamide

수율 55.0%

용매

methylene chloride

반응 조건

후처리

1. 1
   온도The reaction mixture was cooled to RT
2. 2
   세척washed with water (2×5 mL)
3. 3
   건조The organic layer was dried over Na2SO4
4. 4
   농축concentrated
5. 5
   기타the residue was purified by silica gel
6. 6
   세척eluted with 2-10% MeOH/CH3Cl

실험 절차

A mixture of 5-{[2-(6-bromo-pyridin-2-ylamino)-thiazol-5-ylmethyl]-amino}-N-cyclopropyl-2,4-difluoro-benzamide (96 mg, 0.20 mmol) in neat N-methyl piperazine (0.4 mL) was heated to 120° C. in a sealed tube for 5 h. The reaction mixture was cooled to RT, diluted with methylene chloride (5 mL), and washed with water (2×5 mL). The organic layer was dried over Na2SO4, concentrated, and the residue was purified by silica gel eluted with 2-10% MeOH/CH3Cl to give the title compound (53 mg, 55%) as a light yellow solid. (M+H)+=500.

출처