Trifluoroacetic acid → HCID 69085620、化合物

HRID 1023437

反応式

HRID 1023437 の反応式
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

参加物

7

反応物 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

生成物 1

HCID 69085620HCID 69085620、化合物収率 98.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

[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.

後処理

  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

出典と根拠

ORDレコード
ord-09215c7abcba4a68b1ca09ba64fd2bf1
出典データセット
uspto-grants-2014_05
特許番号
US08722709B2

関連ノート

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