Hydrochloric Acid → HCID 11019906、化合物
反応式
[ClH:1].[Cl:2][C:3]1[CH:4]=[C:5]2[C:9](=[CH:10][CH:11]=1)[C:8](=[O:12])[CH2:7][CH2:6]2.ClCl>C(O)(=O)C>[Cl:1][CH:7]1[CH2:6][C:5]2[C:9](=[CH:10][CH:11]=[C:3]([Cl:2])[CH:4]=2)[C:8]1=[O:12]参加物
5
実験手順
Hydrogen chloride gas is passed into a solution of 10.11 g (60 mmoles) of 5-chloro-1-indanone in 50 ml of glacial acetic acid at 10°-15° C. for 30 minutes. 4.25 g (60 mmoles) of condensed chlorine are then allowed to flow slowly into the solution at 10° C. and the mixture is allowed to come gradually to room temperature and is subsequently stirred for 3 hours. After standing overnight, the solution is poured onto ice, the oil which separates out is extracted with acetic acid ethyl ester and the solvent is distilled off under reduced pressure. The oil which remains crystallizes on standing. The product can be recrystallized from petroleum ether and then melts at 63°-66° C.
後処理
- customto flow slowly into the solution at 10° C.
- customto come gradually to room temperature
- waitAfter standing overnight
- additionthe solution is poured onto ice
- extractionthe oil which separates out is extracted with acetic acid ethyl ester
- distillationthe solvent is distilled off under reduced pressure
- customThe oil which remains crystallizes on standing
- customThe product can be recrystallized from petroleum ether
出典と根拠
- ORDレコード
- ord-bed636328b5147e69634a4632a778cba
- 出典データセット
- uspto-grants-1979_11
- 特許番号
- US04174397
反応ノート
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