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

HRID 403557

반응식

HRID 403557 반응식
[F:1][CH:2]([F:5])[CH2:3][OH:4].F[C:7]1[CH:8]=[CH:9][C:10]([N+:17]([O-:19])=[O:18])=[C:11]([CH:16]=1)[C:12]([O:14][CH3:15])=[O:13].CCN(CC)CC.C(N1CCN2CCN(CC(C)C)P1N(CC(C)C)CC2)C(C)C>C1COCC1>[F:1][CH:2]([F:5])[CH2:3][O:4][C:7]1[CH:8]=[CH:9][C:10]([N+:17]([O-:19])=[O:18])=[C:11]([CH:16]=1)[C:12]([O:14][CH3:15])=[O:13]

참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 1361872,2-Difluoroethan-1-olHCID 45712432,8,9-Triisobutyl-2,5,8,9-tetraaza-1-phosphabicyclo(3.3.3)undecaneHCID 51520495-Fluoro-2-nitrobenzoic acid methyl ester

생성물 1

HCID 59587324Methyl 5-(2,2-difluoroethoxy)-2-nitrobenzoate수율 92.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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.

후처리

  1. customThe solvent is evaporated under reduced pressure
  2. additionWater is added
  3. extractionextraction
  4. washThe extract is washed with a 1N aqueous HCl solution, with water
  5. dry with materialIt is dried over MgSO4
  6. filtrationfiltered
  7. customthe solvent is evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-2113f649297a473aaf857ee42f72bf8c
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08748441B2

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