Trifluoroacetic acid → HCID 64128755, 화합물

HRID 1023429노트

반응식

HRID 1023429 반응식
C(OC(=O)[NH:7][C:8]1[CH:13]=[C:12]([CH2:14][C:15]([OH:23])([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH3:16])[CH:11]=[CH:10][N:9]=1)(C)(C)C.FC(F)(F)C(O)=O.CCOC(C)=O.C([O-])(O)=O.[Na+]>C(Cl)Cl.O>[NH2:7][C:8]1[CH:13]=[C:12]([CH2:14][C:15]([C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][CH:22]=2)([OH:23])[CH3:16])[CH:11]=[CH:10][N:9]=1

참가 물질

7

반응물 4

HCID 6422Trifluoroacetic acidHCID 8857Ethyl AcetateHCID 516892Sodium BicarbonateHCID 69083970[4-(2-Hydroxy-2-phenyl-propyl)-pyridin-2-yl]-carbamic acid tert-butyl ester

생성물 1

HCID 64128755HCID 64128755, 화합물수율 122.2%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

To the solution of [4-(2-hydroxy-2-phenyl-propyl)-pyridin-2-yl]-carbamic acid tert-butyl ester (140 mg, 0.43 mmol) in DCM (4 mL) is added trifluoroacetic acid (0.3 mL). The mixture is stirred for 16 hrs at room temperature. Then EtOAc (35 mL) is added followed by the addition of saturated NaHCO3 aquaous solution (15 mL) and water (15 mL). The mixture is stirred for 15 min and the aqueous layer is separated. The aqueous layer is then extracted with EtOAc (2×25 mL). All the organic layers are combined and concentrated to give 120 mg of crude product which is used in the next step without purification.

후처리

  1. stirringThe mixture is stirred for 15 min
  2. customthe aqueous layer is separated
  3. extractionThe aqueous layer is then extracted with EtOAc (2×25 mL)
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-f578ed60473c44e983c1c754598002a7
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722709B2

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