Toluene → 1,4-Dioxaspiro[4.5]decane-8-carbonitrile, 8-(4-fluorophenyl)-

HRID 45186

반응식

HRID 45186 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([C:15]#[N:16])[CH2:13][CH2:12][C:11](=[O:14])[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.C1(C)C=CC(S(O)(=O)=[O:24])=CC=1.[C:28]1([CH3:34])C=CC=CC=1>>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2([C:15]#[N:16])[CH2:9][CH2:10][C:11]3([O:24][CH2:28][CH2:34][O:14]3)[CH2:12][CH2:13]2)=[CH:6][CH:7]=1

참가 물질

4

반응물 3

HCID 1140TolueneHCID 6101p-Toluenesulfonic acidHCID 918051-(4-Fluorophenyl)-4-oxocyclohexanecarbonitrile

생성물 1

HCID 122302421,4-Dioxaspiro[4.5]decane-8-carbonitrile, 8-(4-fluorophenyl)-

실험 절차

15 g of 1-(4-Fluoro-phenyl)-4-oxo-cyclohexanecarbonitrile (12) were dissolved in 500 mL of toluene, then 900 mg of p-toluene sulfonic acid were added and the reaction mixture was heated in a Dean-Stark apparatus for 6 h. The mixture was allowed to cool to room temperature and washed twice with saturated aqueous sodium bicarbonate solution and brine, dried over magnesium sulphate and evaporated to dryness to yield 17.9 g of the desired product. Rt=1.47 min (Method 5). Detected mass: 262.2 (M+H+).

후처리

  1. temperaturethe reaction mixture was heated in a Dean-Stark apparatus for 6 h
  2. washwashed twice with saturated aqueous sodium bicarbonate solution and brine
  3. dry with materialdried over magnesium sulphate
  4. customevaporated to dryness

출처 및 근거

ORD 기록
ord-eb57cc6faa9a46448c8693c8bd34b229
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541449B2

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