Methanol → HCID 54520137、化合物

HRID 1579109ノート

反応式

HRID 1579109 の反応式
[CH:1]1([C:7]2[CH:8]=[CH:9][C:10]3[CH:13]=[C:12]([C:14]([OH:16])=[O:15])[C:11]=3[CH:17]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.O.[CH3:19]O>S(=O)(=O)(O)O>[CH3:19][O:15][C:14]([C:12]1[C:11]2[CH:17]=[C:7]([CH:1]3[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]3)[CH:8]=[CH:9][C:10]=2[CH:13]=1)=[O:16]

参加物

5

反応物 3

HCID 887MethanolHCID 962WaterHCID 21484415HCID 21484415、化合物

生成物 1

HCID 54520137HCID 54520137、化合物

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

A solution of 15 g of 5-cyclohexyl-1-benzocyclobutenecarboxylic acid in 150 ml of absolute methanol and 1.5 ml of concentrated sulphuric acid is boiled for 14 hours under reflux whilst excluding water. The reaction mixture is evaporated in vacuo at 30°C to a volume of approx. 30 ml and the evaporation residue is partitioned between three times 200 ml of ether and twice 200 ml of ice water. The combined organic phases are successively washed with saturated sodium bicarbonate solution and water, dried over sodium sulphate and evaporated in vacuo. Distillation of the evaporation residue in a high vacuum yields 5-cyclohexyl-1-benzocyclobutenecarboxylic acid methyl ester in the fraction boiling at approx. 150°C/0.07 mm Hg.

後処理

  1. temperatureunder reflux
  2. customThe reaction mixture is evaporated in vacuo at 30°C to a volume of approx. 30 ml
  3. customthe evaporation residue is partitioned between three times 200 ml of ether and twice 200 ml of ice water
  4. washThe combined organic phases are successively washed with saturated sodium bicarbonate solution and water
  5. dry with materialdried over sodium sulphate
  6. customevaporated in vacuo
  7. distillationDistillation of the evaporation residue in a high vacuum

出典と根拠

ORDレコード
ord-4496f2d8eda14b498b577a9da4f67c7a
出典データセット
uspto-grants-1976_02
特許番号
US03940434

反応ノート

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