t-Butoxycarbonylamino-3-[2-(4-cyanophenyl)ethoxy]-2-methylbenzene → Amino-3-[2-(4-cyanophenyl)ethoxy]-2-methylbenzene

HRID 325033노트

반응식

HRID 325033 반응식
C(OC([NH:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([O:15][CH2:16][CH2:17][C:18]2[CH:23]=[CH:22][C:21]([C:24]#[N:25])=[CH:20][CH:19]=2)[C:10]=1[CH3:26])=O)(C)(C)C>CCOC(C)=O.Cl>[NH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([O:15][CH2:16][CH2:17][C:18]2[CH:19]=[CH:20][C:21]([C:24]#[N:25])=[CH:22][CH:23]=2)[C:10]=1[CH3:26]

참가 물질

4

반응물 1

HCID 22033517t-Butoxycarbonylamino-3-[2-(4-cyanophenyl)ethoxy]-2-methylbenzene

생성물 1

HCID 22033540Amino-3-[2-(4-cyanophenyl)ethoxy]-2-methylbenzene수율 21.8%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 8857Ethyl Acetate용매

실험 절차

t-Butoxycarbonylamino-3-[2-(4cyanophenyl)ethoxy]-2-methylbenzene (2.69 g, 7.64 mmol; from step (ii) above) were dissolved in EtOAc, pre-saturated with HCl(g), (150 mL) under nitrogen and stirred at room temperature overnight. After evaporation of the solvent the residue was partitioned between 10% aqueous HCl and EtOAc. The aqueous phase was washed with EtOAc, basified with NaOH (2M, aq.) and extracted with EtOAc. The combined organic phases were washed with brine, dried (MgSO4) and the solvent evaporated to afford 0.42 g (19%) of the sub-title compound.

후처리

  1. customAfter evaporation of the solvent the residue
  2. customwas partitioned between 10% aqueous HCl and EtOAc
  3. washThe aqueous phase was washed with EtOAc
  4. extractionextracted with EtOAc
  5. washThe combined organic phases were washed with brine
  6. dry with materialdried (MgSO4)
  7. customthe solvent evaporated

출처 및 근거

ORD 기록
ord-2c5a44f5757b46c7a556afb552752caf
출처 데이터셋
uspto-grants-2001_04
특허 번호
US06221898B1

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