HCID 13234261, 화합물 → HCID 13188692, 화합물
반응식
[CH2:1]([C:3]1([C:9]([CH2:11]C#N)=[O:10])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1)[CH3:2]>Cl>[C:9]([C:3]1([CH2:1][CH3:2])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1)(=[O:10])[CH3:11]참가 물질
3
실험 절차
To 180 g. of (1-ethylcyclohexylcarbonyl)-acetonitrile was added 1 liter of 12 N hydrochloric acid, and the mixture was stirred under reflux for 2.5 hours and was cooled. The mixture was then extracted with one 1000 ml. and one 500 ml. portion of pentane, and the organic layers were combined, dried over magnesium sulfate and concentrated under vacuum at a temperature near 30°. The desired product was found to co-distill, in part, with the solvent, and so the vacuum and temperature were carefully watched to avoid excessive loss of the product, which was identified by its molecular ion in mass spectroscopic analysis, 154. Its boiling point was 44°-45° at 0.4 torr.
후처리
- temperatureunder reflux for 2.5 hours
- temperaturewas cooled
- extractionThe mixture was then extracted with one 1000 ml
- dry with materialdried over magnesium sulfate
- concentrationconcentrated under vacuum at a temperature near 30°
출처 및 근거
- ORD 기록
- ord-87b1cf88f152474981939a34778733b9
- 출처 데이터셋
- uspto-grants-1983_08
- 특허 번호
- US04398044
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