Hydrochloric Acid → HCID 11019906、化合物

HRID 46633ノート

反応式

HRID 46633 の反応式
[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

  1. customto flow slowly into the solution at 10° C.
  2. customto come gradually to room temperature
  3. waitAfter standing overnight
  4. additionthe solution is poured onto ice
  5. extractionthe oil which separates out is extracted with acetic acid ethyl ester
  6. distillationthe solvent is distilled off under reduced pressure
  7. customThe oil which remains crystallizes on standing
  8. 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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