반응 #334000

ord-1183ab9a9abe406ba5a5e4d98980d3f9

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.WAITAfter about ninety minutes
  2. 2
    세척The mixture was washed sequentially with three portions of saturated aqueous sodium bicarbonate and three portions of water
  3. 3
    건조The organic phase was dried over sodium sulfate
  4. 4
    여과filtered
  5. 5
    농축concentrated in vacuo

실험 절차

To a stirred solution of 2.0 g (4.5 mmole) of the title product of Example 2 in 40 ml of cold (ca. 0° ) dichloromethane was added 1.94 g (9.1 mmole) of 81% m-chloroperoxybenzoic acid. After about ninety minutes, 10 ml of saturated aqueous sodium thiosulfate was added. The mixture was washed sequentially with three portions of saturated aqueous sodium bicarbonate and three portions of water. The organic phase was dried over sodium sulfate, filtered, and concentrated in vacuo to give the title compound, m.p. 180°-183°.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04704386uspto-grants-1987_11