반응 #325294

반응 방정식

4-(4-bromo-2,6-difluoroanilino)-7-(1-(tert-butoxycarbonyl)piperidin-4-ylmethoxy)-6-methoxyquinazoline

TFA

→

4-(4-bromo-2,6-difluoroanilino)-6-methoxy-7-(piperidin-4-ylmethoxy)quinazoline

수율 23.0%

용매

methylene chloride

반응 조건

후처리

1. 1
   기타The volatiles were removed under vacuum
2. 2
   추출was extracted with methylene chloride
3. 3
   세척The organic layer was washed with water, brine
4. 4
   건조dried (MgSO4)
5. 5
   기타the volatiles were removed by evaporation
6. 6
   기타The residue was triturated with ether
7. 7
   기타dried under vacuum

실험 절차

A solution of 4-(4-bromo-2,6-difluoroanilino)-7-(1-(tert-butoxycarbonyl)piperidin-4-ylmethoxy)-6-methoxyquinazoline (578 mg, 1 mmol) in methylene chloride (10 ml) containing TFA (4 ml) was stirred at ambient temperature for 2 hours. The volatiles were removed under vacuum and the residue was suspended in water. The aqueous layer was adjusted to approximately pH10 and was extracted with methylene chloride. The organic layer was washed with water, brine, dried (MgSO4) and the volatiles were removed by evaporation. The residue was triturated with ether and dried under vacuum to give 4-(4-bromo-2,6-difluoroanilino)-6-methoxy-7-(piperidin-4-ylmethoxy)quinazoline (110 mg, 23%).

출처