3-[3-(4-Ethyl-2,2,7-trimethyl-3-oxo-3,4-dihydro-2H-benzo[1,4]oxazin-6-yl)-4-trifluoromethoxy-phenyl]-acrylic acid tert-butyl ester → 3-[3-(4-Ethyl-2,2,7-trimethyl-3-oxo-3,4-dihydro-2H-benzo[1,4]oxazin-6-yl)-4-trifluoromethoxy-phenyl]-acrylic acid

HRID 2239242노트

반응식

HRID 2239242 반응식
C([O:5][C:6](=[O:36])[CH:7]=[CH:8][C:9]1[CH:14]=[CH:13][C:12]([O:15][C:16]([F:19])([F:18])[F:17])=[C:11]([C:20]2[C:21]([CH3:35])=[CH:22][C:23]3[O:28][C:27]([CH3:30])([CH3:29])[C:26](=[O:31])[N:25]([CH2:32][CH3:33])[C:24]=3[CH:34]=2)[CH:10]=1)(C)(C)C>ClCCl.FC(F)(F)C(O)=O>[CH2:32]([N:25]1[C:24]2[CH:34]=[C:20]([C:11]3[CH:10]=[C:9]([CH:8]=[CH:7][C:6]([OH:36])=[O:5])[CH:14]=[CH:13][C:12]=3[O:15][C:16]([F:19])([F:17])[F:18])[C:21]([CH3:35])=[CH:22][C:23]=2[O:28][C:27]([CH3:30])([CH3:29])[C:26]1=[O:31])[CH3:33]

참가 물질

4

반응물 1

HCID 685832583-[3-(4-Ethyl-2,2,7-trimethyl-3-oxo-3,4-dihydro-2H-benzo[1,4]oxazin-6-yl)-4-trifluoromethoxy-phenyl]-acrylic acid tert-butyl ester

생성물 1

HCID 685828733-[3-(4-Ethyl-2,2,7-trimethyl-3-oxo-3,4-dihydro-2H-benzo[1,4]oxazin-6-yl)-4-trifluoromethoxy-phenyl]-acrylic acid수율 100%

시약·촉매·용매 2

HCID 6344Dichloromethane용매HCID 6422Trifluoroacetic acid용매

실험 절차

A solution of Compound 1E (1.71 g, 3.4 mmol) in 15 mL of dichloromethane and 5 mL of trifluoroacetic acid was stirred at room temperature overnight. The reaction mixture was then concentrated on the rotary evaporator and redissolved in 20 mL of diethyl ether. To this solution, hexanes were added to give a cloudy solution from which 1.5 g (100%) of product precipitated out as a white solid (Compound 1). MS (electrospray): mass calculated for C23H22F3NO5, 449.15; m/z found 462.3, [M+H]+.

후처리

  1. concentrationThe reaction mixture was then concentrated on the rotary evaporator
  2. dissolutionredissolved in 20 mL of diethyl ether
  3. additionTo this solution, hexanes were added

출처 및 근거

ORD 기록
ord-5a05085655f84e11bd6d3dd074fcfe02
출처 데이터셋
uspto-grants-2010_05
특허 번호
US07723326B2

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