Trifluoroacetic acid → (R)-1-(2-fluoro-6-(trifluoromethyl)benzyl)-3-(2-amino-2-phenylethyl)-5-(2-chlorophenyl)pyrimidine-2,4(1H,3H)-dione

HRID 1744292ノート

反応式

HRID 1744292 の反応式
C(OC([NH:8][C@H:9]([C:38]1[CH:43]=[CH:42][CH:41]=[CH:40][CH:39]=1)[CH2:10][N:11]1[C:16](=[O:17])[C:15]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[Cl:24])=[CH:14][N:13]([CH2:25][C:26]2[C:31]([C:32]([F:35])([F:34])[F:33])=[CH:30][CH:29]=[CH:28][C:27]=2[F:36])[C:12]1=[O:37])=O)(C)(C)C.C(O)(C(F)(F)F)=O>C(Cl)Cl>[NH2:8][C@H:9]([C:38]1[CH:39]=[CH:40][CH:41]=[CH:42][CH:43]=1)[CH2:10][N:11]1[C:16](=[O:17])[C:15]([C:18]2[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=2[Cl:24])=[CH:14][N:13]([CH2:25][C:26]2[C:31]([C:32]([F:34])([F:33])[F:35])=[CH:30][CH:29]=[CH:28][C:27]=2[F:36])[C:12]1=[O:37]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 210183933-[2(R)-{tert-butoxycarbonyl-amino}-2-phenylethyl]-5-(2-chlorophenyl)-1-[2-fluoro-6-(trifluoromethyl)benzyl]-pyrimidine-2,4(1H,3H)-dione

生成物 1

HCID 21018389(R)-1-(2-fluoro-6-(trifluoromethyl)benzyl)-3-(2-amino-2-phenylethyl)-5-(2-chlorophenyl)pyrimidine-2,4(1H,3H)-dione収率 100.7%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of compound 2e (0.144 g, 0.23 mmol) in DCM (1 mL) was added TFA (0.5 mL, 6.5 mmol) and the mixture was stirred at room temperature for 1.5 hours. After concentration, the residue was taken up in DCM and sat'd aq. NaHCO3 was added. The aq. layer was extracted with DCM. Combined organic extracts were dried over Na2SO4 and concentrated to give compound 1c (0.12 g). MS (CI) m/z 518.0, 520.1 (MH+).

後処理

  1. concentrationAfter concentration
  2. additionwas added
  3. extractionThe aq. layer was extracted with DCM
  4. dry with materialCombined organic extracts were dried over Na2SO4
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-d4908d7826124288960192a5920eb844
出典データセット
uspto-grants-2006_03
特許番号
US07015226B2

反応ノート

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