반응 #93239

ord-24eef094ff484bfca05ec2cb6d8ee2a1

용매

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도The reaction mixture was cooled with an ice-bath
  2. 2
    기타The ether layer was decanted
  3. 3
    세척washed with brine
  4. 4
    기타dried
  5. 5
    기타evaporated to dryness
  6. 6
    기타The resulting oily residue was chromatographed on silica gel (10% EtOAc/hexane)

실험 절차

Potassium tert. butoxide (1.3 gm) was added to a solution of 5-acetoxy-12H-benzo[a]phenothiazine (from Example 1) (2.0 gm) and methyl iodide (4 ml) in DMF (20 ml). The reaction mixture was cooled with an ice-bath and stirred for 15 minutes. Diethyl ether (100 ml) was added to the reaction mixture followed by brine (100 ml). The ether layer was decanted, washed with brine, dried and evaporated to dryness. The resulting oily residue was chromatographed on silica gel (10% EtOAc/hexane) to afford 5-methoxy-12-methyl-12H-benzo[a]phenothiazine.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04611056uspto-grants-1986_09