반응 #167654

반응 방정식

2,2-difluoroethanol

methyl 5-fluoro-2-nitrobenzoate

NEt3

2,8,9-triisobutyl-2,5,8,9-tetraaza-1-phosphabicyclo[3.3.3]undecane

→

expected product

수율 92.5%

Methyl 5-(2,2-difluoroethoxy)-2-nitrobenzoate

수율 92.5%

용매

THF

반응 조건

후처리

1. 1
   기타The solvent is evaporated under reduced pressure
2. 2
   workup.ADDITIONWater is added
3. 3
   추출extraction
4. 4
   세척The extract is washed with a 1N aqueous HCl solution, with water
5. 5
   건조It is dried over MgSO4
6. 6
   여과filtered
7. 7
   기타the solvent is evaporated under reduced pressure

실험 절차

8.53 g of 2,2-difluoroethanol are added to a solution of 17.31 g of methyl 5-fluoro-2-nitrobenzoate, 9.64 g of NEt3 and 32.71 g of 2,8,9-triisobutyl-2,5,8,9-tetraaza-1-phosphabicyclo[3.3.3]undecane in 250 ml of anhydrous THF. The mixture is stirred at AT for 30 min. The solvent is evaporated under reduced pressure. Water is added and extraction is carried out with AcOEt. The extract is washed with a 1N aqueous HCl solution, with water and then with a saturated NaCl solution. It is dried over MgSO4 and filtered, and the solvent is evaporated under reduced pressure to give 21 g of the expected product.

출처