Methanol → HCID 54520137, 화합물

HRID 1579109노트

반응식

HRID 1579109 반응식
[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]

참가 물질

5

반응물 3

HCID 887MethanolHCID 962WaterHCID 21484415HCID 21484415, 화합물

생성물 1

HCID 54520137HCID 54520137, 화합물

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-4496f2d8eda14b498b577a9da4f67c7a
출처 데이터셋
uspto-grants-1976_02
특허 번호
US03940434

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