Aluminum(III) Chloride → HCID 12395586、化合物

HRID 597007ノート

反応式

HRID 597007 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-2-isopropyl-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 1 hour and cooled. The heptane is decanted from the reaction mixture and the solid residue is poured 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 1 hour
  2. temperaturecooled
  3. customThe heptane is decanted from the reaction mixture
  4. additionthe solid residue is poured into water (300 ml.) and concentrated hydrochloric acid (20 ml.)
  5. extractionThe crude product is extracted into ether (300 ml.)
  6. washwashed with water
  7. dry with materialdried over magnesium sulfate
  8. distillationdistilled to a volume of 100 ml
  9. additionand treated with hexane (100 ml.)

出典と根拠

ORDレコード
ord-93bbf51cc54a4992bb442b2c80000ce2
出典データセット
uspto-grants-1977_03
特許番号
US04012524

反応ノート

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