Trifluoroacetic acid → HCID 69085620, 화합물

HRID 1023437

반응식

HRID 1023437 반응식
C(OC(=O)[NH:7][C:8]1[CH:13]=[C:12]([CH2:14][C:15](O)([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)[C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH3:22])[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>[C:23]1([C:15]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH3:22])=[CH:14][C:12]2[CH:11]=[CH:10][N:9]=[C:8]([NH2:7])[CH:13]=2)[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1

참가 물질

7

반응물 4

HCID 6422Trifluoroacetic acidHCID 8857Ethyl AcetateHCID 516892Sodium BicarbonateHCID 69675871[4-(2-Hydroxy-2-phenyl-2-o-tolyl-ethyl)-pyridin-2-yl]-carbamic acid tert-butyl ester

생성물 1

HCID 69085620HCID 69085620, 화합물수율 98.5%

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

[4-(2-Hydroxy-2-phenyl-2-o-tolyl-ethyl)-pyridin-2-yl]-carbamic acid tert-butyl ester (361 mg, 0.89 mmol) is dissolved in DCM (4 mL) and trifluoroacetic acid (2.0 mL) is added. After the mixture is stirred for 16 hrs, EtOAc (55 mL) is added followed by the addition of saturated NaHCO3 aqueous solution (15 mL) and water (35 mL). The mixture is stirred for another 15 min and the aqueous layer is separated. The aqueous layer is then extracted with EtOAc (2×35 mL) and all the organic layers are combined and concentrated to give 251 mg of the crude product which is used in the next step without purification.

후처리

  1. stirringThe mixture is stirred for another 15 min
  2. customthe aqueous layer is separated
  3. extractionThe aqueous layer is then extracted with EtOAc (2×35 mL) and all the organic layers
  4. concentrationconcentrated

출처 및 근거

ORD 기록
ord-09215c7abcba4a68b1ca09ba64fd2bf1
출처 데이터셋
uspto-grants-2014_05
특허 번호
US08722709B2

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