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

HRID 2164057

반응식

HRID 2164057 반응식
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

참가 물질

6

반응물 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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매2회HCID 312751,4-Dioxane용매

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-30bf2188b06042f38f466cc7ff5013fb
출처 데이터셋
uspto-grants-1979_01
특허 번호
US04137323

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