反応 #76848

ord-082b9be9dcda465b9bdf248233b3d72a

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    濃縮The mixture was then concentrated in vacuo
  2. 2
    抽出extracted three times with with CH2Cl2
  3. 3
    乾燥the combined organic phases were dried over anhydrous MgSO4
  4. 4
    ろ過filtered
  5. 5
    濃縮concentrated

実験手順

To a solution of 1-[(3,4-Dimethoxy-benzyl)-6,7-dimethoxy-1,2,3,4-tetrahydro-naphthalen-2-yl]-phenyl-acetic acid methyl ester (5.85 g, 0.011 mmol) in a mixture dioxane/MeOH (4/3) (160 ml) was added dropwise 2M NaOH(aq) (81 ml). The resulting mixture was stirred at RT for 20 h under nitrogen. The mixture was then concentrated in vacuo, combined with water and AcOEt. The aqueous phase was acidified until pH 1 with 2N HCl, extracted three times with with CH2Cl2, the combined organic phases were dried over anhydrous MgSO4, filtered and concentrated to give the titled product (5.55 g, 97%) as yellow-green crystals.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US06703392B2uspto-grants-2004_03