Aluminum(III) Chloride → HCID 12395586、化合物

HRID 1287439ノート

反応式

HRID 1287439 の反応式
[CH3:1][C:2]1([CH:16]([CH3:18])[CH3:17])[CH2:10][C:9]2[C:4](=[C:5]([Cl:14])[C:6]([Cl:13])=[C:7]([O:11]C)[CH:8]=2)[C:3]1=[O:15].[Cl-].[Al+3].[Cl-].[Cl-]>CCCCCCC>[CH3:1][C:2]1([CH:16]([CH3:18])[CH3:17])[CH2:10][C:9]2[C:4](=[C:5]([Cl:14])[C:6]([Cl:13])=[C:7]([OH:11])[CH:8]=2)[C:3]1=[O:15]

参加物

4

反応物 2

HCID 6451240Aluminum(III) ChlorideHCID 12395564HCID 12395564、化合物

生成物 1

HCID 12395586HCID 12395586、化合物

試薬・触媒・溶媒 1

HCID 8900Heptane溶媒

実験手順

A stirred suspension of 2-methyl-2isopropyl-5-methoxy-6,7-dichloro-1-indanone (7.0 g., 0.0244 mole) and aluminum chloride (9.0 g., 0.068 mole) in heptane (400 ml.) is refluxed for one hour and cooled. The heptane is decanted from the reaction mixture and the solid residue is poiured into water (300 ml.) and concentrated hydrochloric acid (20 ml.). The crude product is extracted into ether (300 ml.), washed with water, dried over magnesium sulfate, distilled to a volume of 100 ml. and treated with hexane (100 ml.). The 2-methyl-2-isopropyl-5-hydroxy-6,7-dichloro-1-indanone which separates (6.5 g.) melts at 215° C.

後処理

  1. temperatureis refluxed for one hour
  2. temperaturecooled
  3. customThe heptane is decanted from the reaction mixture
  4. extractionThe crude product is extracted into ether (300 ml.)
  5. washwashed with water
  6. dry with materialdried over magnesium sulfate
  7. distillationdistilled to a volume of 100 ml
  8. additionand treated with hexane (100 ml.)

出典と根拠

ORDレコード
ord-3c661a221db741c682012db31d99cb62
出典データセット
uspto-grants-1976_10
特許番号
US03984465

反応ノート

読み込み中…