Sulfuric Acid → 6,7-Dihydro-2-methyl-4(5H) benzofuranone

HRID 1252794

反応式

HRID 1252794 の反応式
OS(O)(=O)=O.O[C:7]1[CH2:12][CH2:11][CH2:10][C:9](=[O:13])[C:8]=1[CH2:14][C:15](=[O:17])[CH3:16]>C(Cl)Cl>[CH3:16][C:15]1[O:17][C:7]2[CH2:12][CH2:11][CH2:10][C:9](=[O:13])[C:8]=2[CH:14]=1

参加物

4

実験手順

To a solution of conc. H2SO4 (300 ml) cooled in an ice-bath was added a solution of 3-hydroxy-2(2-oxopropyl)-2-cyclohexene-1-one (190 g in 300 ml CH2Cl2). Upon completion of addition, the mixture was stirred at ambient temperature for about 1 hour. The mixture was then slowly poured into 3 l ice water, and then about 1 l of CH2Cl2 was added. The layers are separated and the aqueous layer extracted thrice with CH2Cl2 and the combined CH2Cl2 layers again extracted thrice with water. The CH2Cl2 layer washed thrice with dilute aqueous NaHCO3, then once with water and dried (MgSO4). Concentration in vacuo afford an orange oil.

後処理

  1. additionUpon completion of addition
  2. customThe layers are separated
  3. extractionthe aqueous layer extracted thrice with CH2Cl2
  4. washThe CH2Cl2 layer washed thrice with dilute aqueous NaHCO3
  5. dry with materialonce with water and dried (MgSO4)
  6. concentrationConcentration in vacuo
  7. customafford an orange oil

出典と根拠

ORDレコード
ord-27938cde0583418c82206b978208bd88
出典データセット
uspto-grants-1988_05
特許番号
US04745222

関連ノート

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