HCID 13234261、化合物 → HCID 13188692、化合物
反応式
[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]参加物
3
実験手順
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.
後処理
- 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°
出典と根拠
- ORDレコード
- ord-87b1cf88f152474981939a34778733b9
- 出典データセット
- uspto-grants-1983_08
- 特許番号
- US04398044
反応ノート
読み込み中…