反応 #10197

ord-99b5561f14694dee9f68132e67b69d9b

反応方程式

O=C([O-])O.[Na+]
NaHCO3
O=C(N1CC2CC(C1)c1ccccc12)C(F)(F)F
1-(10-Aza-tricyclo[6.3.1.02,7]dodeca-2(7),3,5-trien-10-yl)-2,2,2-trifluoro-ethanone
CC(=O)Cl
AcCl
[Al+3].[Cl-].[Cl-].[Cl-]
aluminum chloride
CC(=O)c1ccc2c(c1)C1CC2CN(C(=O)C(F)(F)F)C1
1-(4-Acetyl-10-aza-tricyclo[6.3.1.02,7]dodeca-2(7),3,5-trien-10-yl)-2,2,2-trifluoro-ethanone

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    workup.STIRRINGAfter stirring 20 minutes the mixture
  2. 2
    抽出was extracted with CH2Cl2 (3×30 mL)
  3. 3
    その他The organic layer was dried through a cotton plug
  4. 4
    濃縮then concentrated to a orange-yellow oil (255 mg, 86%)

実験手順

1-(10-Aza-tricyclo[6.3.1.02,7]dodeca-2(7),3,5-trien-10-yl)-2,2,2-trifluoro-ethanone (253 mg, 1.0 mmol) and AcCl (0.68 mL, 10 mmol) were dissolved in DCE (3 mL) and treated with aluminum chloride (AlCl3) (667 mg, 5.0 mmol). The resulting yellow mixture was stirred for 30 minutes then poured over ice and saturated aqueous NaHCO3 solution. After stirring 20 minutes the mixture was extracted with CH2Cl2 (3×30 mL). The organic layer was dried through a cotton plug then concentrated to a orange-yellow oil (255 mg, 86%).

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07091372B2uspto-grants-2006_08