Aluminum(III) Chloride → HCID 12395586, 화합물

HRID 597007노트

반응식

HRID 597007 반응식
[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]

참가 물질

4

반응물 2

HCID 6451240Aluminum(III) ChlorideHCID 12395564HCID 12395564, 화합물

생성물 1

HCID 12395586HCID 12395586, 화합물

시약·촉매·용매 1

HCID 8900Heptane용매

실험 절차

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.

후처리

  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.)

출처 및 근거

ORD 기록
ord-93bbf51cc54a4992bb442b2c80000ce2
출처 데이터셋
uspto-grants-1977_03
특허 번호
US04012524

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