HCID 178448752、化合物 → HCID 178520821、化合物

HRID 2242147ノート

反応式

HRID 2242147 の反応式
C([N:5]1[C:9]([NH:10][C:11](=[O:19])[CH2:12][CH2:13][N:14]2[CH:18]=[CH:17][CH:16]=[N:15]2)=[CH:8][C:7]([C@@H:20]2[CH2:23][C@H:22]([O:24][C:25](=[O:34])[NH:26][CH2:27][CH:28]3[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]3)[CH2:21]2)=[N:6]1)(C)(C)C>C(O)(C(F)(F)F)=O>[N:14]1([CH2:13][CH2:12][C:11]([NH:10][C:9]2[NH:5][N:6]=[C:7]([C@@H:20]3[CH2:21][C@H:22]([O:24][C:25](=[O:34])[NH:26][CH2:27][CH:28]4[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]4)[CH2:23]3)[CH:8]=2)=[O:19])[CH:18]=[CH:17][CH:16]=[N:15]1

参加物

3

反応物 1

HCID 178448752HCID 178448752、化合物

生成物 1

HCID 178520821HCID 178520821、化合物

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

A solution of cyclohexylmethyl-carbamic acid cis-3-[1-tert-butyl-5-(3-pyrazol-1-yl-propionylamino)-1H-pyrazol-3-yl]-cyclobutyl ester from Step A (122 mg) in TFA (2 mL) was heated at 120° C. in a microwave apparatus for 10 min. The solution was concentrated and the residue was dissolved in EtOAc. The resulting solution was washed sequentially with portions of saturated aqueous NaHCO3 solution and saturated aqueous NaCl solution. The organic layer was dried over Na2SO4 and concentrated. The residue was purified by silica gel chromatography to afford the title product as a white solid. MS (M+H)+=415.5.

後処理

  1. concentrationThe solution was concentrated
  2. dissolutionthe residue was dissolved in EtOAc
  3. washThe resulting solution was washed sequentially with portions of saturated aqueous NaHCO3 solution and saturated aqueous NaCl solution
  4. dry with materialThe organic layer was dried over Na2SO4
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel chromatography

出典と根拠

ORDレコード
ord-750775f380f14ffd8839029ab170e442
出典データセット
uspto-grants-2010_03
特許番号
US07671072B2

反応ノート

読み込み中…