반응 #1436570

ord-eb43a9c92c3f4ff088654273cf124f81

반응 방정식

CN(C)C1(c2ccccc2)CCC(=O)CC1
4-dimethylamino-4-phenylcyclohexanone
O=B[O-].[Na+]
sodium boranate
O=P([O-])([O-])[O-]
phosphate
CN(C)C1(c2ccccc2)CCC(O)CC1
4-dimethylamino-4-phenylcyclohexanol
수율 81.3%

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    온도while cooling with an ice bath
  2. 2
    농축the mixture was concentrated
  3. 3
    기타The phases were separated
  4. 4
    추출extracted three times
  5. 5
    건조The combined organic phases were dried over sodium sulfate
  6. 6
    여과filtered
  7. 7
    농축concentrated

실험 절차

3.35 g of 4-dimethylamino-4-phenylcyclohexanone were suspended in 25 ml of isopropanol; 620 mg of sodium boranate were added, while cooling with an ice bath, and stirring was carried out overnight at room temperature. 6.5 ml of phosphate buffer (pH 7, Merck-Darmstadt) were added dropwise and the mixture was concentrated. The residue was taken up in 10 ml of water and 20 ml of diethyl ether and rendered alkaline with potassium hydroxide. The phases were separated and extracted three times using 15 ml of diethyl ether each time. The combined organic phases were dried over sodium sulfate, filtered and concentrated. 2.75 g of 4-dimethylamino-4-phenylcyclohexanol were obtained.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07211694B2uspto-grants-2007_05