반응 #1242822

ord-bcc2d5ee189e42939b6ab27fa5748507

용매

반응 조건

온도
48°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타fitted with a condenser
  2. 2
    기타The dark brown mixture is oxygenated for 100 minutes at room temperature
  3. 3
    기타10 minutes
  4. 4
    기타is reheated to 50° C.
  5. 5
    기타the flow of oxygen is terminated 2 hours later

실험 절차

Oxygen is passed into a mixture of N-(4,5,6,7-tetrahydrobenzo[b]thien-4-yl)acetamide (1.0 g; 5.13 m mole), cobaltous acetate (0.25 g; 1.4 m mole), cobaltous bromide tetrahydrate (0.32 g; 1.1 m mole), isobutyric acid (20 ml) and water (0.2 ml) in a sintered glass funnel fitted with a condenser and thermometer, via the stem of the funnel. The dark brown mixture is oxygenated for 100 minutes at room temperature, then heated briefly to 48° C. After 2 hours and 10 minutes, the mixture is reheated to 50° C. and the flow of oxygen is terminated 2 hours later. The mixture is then worked up as described in Example 1 to attain a 37% yield of the title compound.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04332724uspto-grants-1982_06