Hydrochloric Acid → 1,4-Dioxaspiro[4.5]decane-8-carboxylic acid, 8-(4-fluorophenyl)-

HRID 2370294노트

반응식

HRID 2370294 반응식
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([C:18]#N)[CH2:17][CH2:16][C:11]3([O:15][CH2:14][CH2:13][O:12]3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1.[OH-:20].[K+].[OH2:22].Cl>C(O)CO>[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2([C:18]([OH:22])=[O:20])[CH2:17][CH2:16][C:11]3([O:15][CH2:14][CH2:13][O:12]3)[CH2:10][CH2:9]2)=[CH:4][CH:3]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 14797Potassium HydroxideHCID 122302421,4-Dioxaspiro[4.5]decane-8-carbonitrile, 8-(4-fluorophenyl)-

생성물 1

HCID 122302461,4-Dioxaspiro[4.5]decane-8-carboxylic acid, 8-(4-fluorophenyl)-

시약·촉매·용매 1

HCID 174Ethylene Glycol용매

실험 절차

30.1 g of 8-(4-Fluoro-phenyl)-1,4-dioxa-spiro[4.5]decane-8-carbonitrile (74) were dissolved in 91 mL of ethylene glycol. 19.4 g of powdered potassium hydroxide were added and the mixture was heated to reflux until conversion was complete. The mixture was allowed to cool down to room temperature and poured into 300 mL of water. The pH was adjusted to 4 by addition of 2N HCl and the aqueous layer was extracted With ethyl acetate. The organic layer was extracted with brine, dried over magnesium sulfate and evaporated to dryness to give 29.85 g of the desired product. Rt=1.81 min (Method B). Detected mass: 281.2 (M+H+).

후처리

  1. temperaturethe mixture was heated
  2. temperatureto reflux until conversion
  3. extractionthe aqueous layer was extracted With ethyl acetate
  4. extractionThe organic layer was extracted with brine
  5. dry with materialdried over magnesium sulfate
  6. customevaporated to dryness

출처 및 근거

ORD 기록
ord-e3be8928a63b4a21a7114ee0bb840827
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08710077B2

반응 노트

불러오는 중…