Trifluoroacetic acid → HCID 64128755、化合物

HRID 1023429ノート

反応式

HRID 1023429 の反応式
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

参加物

7

反応物 4

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

生成物 1

HCID 64128755HCID 64128755、化合物収率 122.2%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-f578ed60473c44e983c1c754598002a7
出典データセット
uspto-grants-2014_05
特許番号
US08722709B2

反応ノート

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