Hydrochloric Acid → 4-(9,10-dihydro-4-oxo-4H-benzo[4,5]cyclohepta[1,2-b]thiophen-2-yl)-4-oxobutyric acid

HRID 972216

反応式

HRID 972216 の反応式
C[O:2][C:3](=[O:23])[CH2:4][CH2:5][C:6]([C:8]1[S:12][C:11]2[CH2:13][CH2:14][C:15]3[CH:22]=[CH:21][CH:20]=[CH:19][C:16]=3[C:17](=[O:18])[C:10]=2[CH:9]=1)=[O:7].[OH-].[K+].Cl>O1CCOCC1.O>[O:18]=[C:17]1[C:10]2[CH:9]=[C:8]([C:6](=[O:7])[CH2:5][CH2:4][C:3]([OH:23])=[O:2])[S:12][C:11]=2[CH2:13][CH2:14][C:15]2[CH:22]=[CH:21][CH:20]=[CH:19][C:16]1=2

参加物

6

反応物 3

HCID 313Hydrochloric AcidHCID 14797Potassium HydroxideHCID 537502014-(9,10-dihydro-4-oxo-4H-benzo[4,5]cyclohepta[1,2-b]thiophen-2-yl)-4-oxobutyric acid methyl ester

生成物 1

HCID 227501404-(9,10-dihydro-4-oxo-4H-benzo[4,5]cyclohepta[1,2-b]thiophen-2-yl)-4-oxobutyric acid

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 312751,4-Dioxane溶媒

実験手順

A solution of 3.0 g of 4-(9,10-dihydro-4- oxo-4H-benzo[4,5]cyclohepta[1,2-b]thiophen-2-yl)-4- oxobutyric acid methyl ester and 1.5 g of potassium hydroxide in 60 cc of dioxane and 30 cc of water is stirred at room temperature for 3 hours, dilution is effected with 200 cc of water and the pH of the solution is adjusted to 1 with concentrated hydrochloric acid at 10°-15°. The resulting title compound is extracted with methylene chloride, the organic solution is washed with water, dried over magnesium sulphate, concentrated by evaporation, and the title compound is recrystallized from dimethyl formamide/acetone. M.P. 167°-168°.

後処理

  1. extractionThe resulting title compound is extracted with methylene chloride
  2. washthe organic solution is washed with water
  3. dry with materialdried over magnesium sulphate
  4. concentrationconcentrated by evaporation
  5. customthe title compound is recrystallized from dimethyl formamide/acetone

出典と根拠

ORDレコード
ord-cc82418122684b4a9edca1b3b527809f
出典データセット
uspto-grants-1977_10
特許番号
US04052412

関連ノート

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