Trifluoroacetic acid → HCID 68487595, 화합물

HRID 1875099노트

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HRID 1875099 반응식
C(O)(C(F)(F)F)=O.CC([N:12]([CH2:16][C:17]1[CH:22]=[CH:21][C:20]([CH2:23][CH3:24])=[C:19]([O:25][C:26]2[CH:31]=[C:30]([C:32]#[N:33])[CH:29]=[C:28]([Cl:34])[CH:27]=2)[C:18]=1[F:35])C(=O)[O-])(C)C>C(Cl)Cl>[NH2:12][CH2:16][C:17]1[C:18]([F:35])=[C:19]([O:25][C:26]2[CH:31]=[C:30]([CH:29]=[C:28]([Cl:34])[CH:27]=2)[C:32]#[N:33])[C:20]([CH2:23][CH3:24])=[CH:21][CH:22]=1

참가 물질

4

반응물 2

HCID 6422Trifluoroacetic acidHCID 867616521,1-Dimethylethyl({3-[(3-chloro-5-cyanophenyl)oxy]-4-ethyl-2-fluorophenyl}methyl)carbamate

생성물 1

HCID 68487595HCID 68487595, 화합물수율 101%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

TFA (1.903 ml, 24.70 mmol) was added to a solution of 1,1-dimethylethyl({3-[(3-chloro-5-cyanophenyl)oxy]-4-ethyl-2-fluorophenyl}methyl)carbamate (0.5 g, 1.235 mmol) in DCM (30 mL) at RT under an atmosphere of nitrogen. After 16 h, the solution was concentrated under vacuum. Saturated NaHCO3 solution (100 mL) and ethyl acetate (100 mL) were added and the mixture was stirred for 1 h. The organic layer was separated, washed with water (100 mL), brine (100 mL), dried over Na2SO4, filtered and concentrated to give the title compound (0.38 g, >99%) as a brown oil. 1H NMR (400 MHz, CHLOROFORM-d) δ ppm 7.29-7.33 (m, 1H), 7.21-7.27 (m, 1H), 7.13 (t, 1H), 7.09 (d, 1H), 6.98 (s, 1H), 3.92 (s, 2H), 2.54 (d, 2H), 1.54 (d, 2H), 1.13-1.19 (m, 3H).

후처리

  1. concentrationthe solution was concentrated under vacuum
  2. additionSaturated NaHCO3 solution (100 mL) and ethyl acetate (100 mL) were added
  3. customThe organic layer was separated
  4. washwashed with water (100 mL), brine (100 mL)
  5. dry with materialdried over Na2SO4
  6. filtrationfiltered
  7. concentrationconcentrated

출처 및 근거

ORD 기록
ord-887f798b9c42427f8e7cd2b25ba7f8c9
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08304419B2

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