Phosphorus pentachloride → HCID 68568880、化合物
反応式
[CH3:1][C:2]12[O:11][CH:8]([CH2:9][CH2:10]1)[CH:7]1[CH:3]2[C:4](=[O:13])[CH2:5][C:6]1=O.P(Cl)(Cl)(Cl)(Cl)[Cl:15]>C(Cl)(Cl)Cl>[Cl:15][C:6]1[CH:7]2[CH:3]([C:2]3([CH3:1])[O:11][CH:8]2[CH2:9][CH2:10]3)[C:4](=[O:13])[CH:5]=1参加物
4
実験手順
To a solution of 1-methyl-10-oxa-tricyclo[5.2.1.0*2,6*]decane-3,5-dione (3 g, 16.6 mmol) in chloroform (8 ml) is added PCl5 portionwise. The reaction mixture is stirred and heated at reflux for 5 hours. The reaction mixture is evaporated to dryness The crude product is purified by flash chromatography on silica gel to give 5-chloro-1-methyl-10-oxa-tricyclo[5.2.1.0*2,6*]dec-4-en-3-one (1.39 g).
後処理
- temperatureheated
- temperatureat reflux for 5 hours
- customThe reaction mixture is evaporated to dryness The crude product
- customis purified by flash chromatography on silica gel
出典と根拠
- ORDレコード
- ord-d4c209656121418b9e37ee965c078d8b
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08530667B2
反応ノート
読み込み中…