反応 #595388

ord-d632bfd73feb4e52b46375d4c90a0c8a

反応方程式

O=C(OCc1ccccc1)c1ccc(-c2nn(C(=O)c3c(Cl)cccc3C(F)(F)F)c3ccccc23)cc1CO
benzyl 4-(1-(2-chloro-6-(trifluoromethyl)benzoyl)-1H-indazol-3-yl)-2-(hydroxymethyl)benzoate
CC(=O)OI1(OC(C)=O)(OC(C)=O)OC(=O)c2ccccc21
Dess-Martin periodinane
O=Cc1cc(-c2nn(C(=O)c3c(Cl)cccc3C(F)(F)F)c3ccccc23)ccc1C(=O)OCc1ccccc1
benzyl 4-(1-(2-chloro-6-(trifluoromethyl)benzoyl)-1H-indazol-3-yl)-2-formylbenzoate

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    抽出extracted with DCM
  2. 2
    洗浄The combined organic layers were washed with brine
  3. 3
    乾燥dried over Na2SO4
  4. 4
    濃縮concentrated
  5. 5
    その他The resulting crude oil was used in the next step without further purification

実験手順

To a mixture of benzyl 4-(1-(2-chloro-6-(trifluoromethyl)benzoyl)-1H-indazol-3-yl)-2-(hydroxymethyl)benzoate (G-3) (0.4 g, 0.71 mmol) in DCM (10 mL) was added Dess-Martin periodinane (0.45 g, 1.07 mmol), and the mixture was stirred at rt for 24 h. The mixture was diluted with H2O and extracted with DCM. The combined organic layers were washed with brine, dried over Na2SO4 and concentrated. The resulting crude oil was used in the next step without further purification. LCMS (ESI)′ calc'd for C30H19ClF3N2O4 [M+H]+: 563. found: 563.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US09095583B2uspto-grants-2015_08