Hydrochloric Acid → 7-(4-Methyl-2-thienyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid

HRID 1978605ノート

反応式

HRID 1978605 の反応式
Cl.[CH3:2][C:3]1[CH:4]=[C:5]([C:8]2[CH:9]=[CH:10][C:11]3[S:17](=[O:19])(=[O:18])[CH2:16][CH2:15][C:14]([C:20]([O:22]C)=[O:21])=[CH:13][C:12]=3[CH:24]=2)[S:6][CH:7]=1>COCCOC>[CH3:2][C:3]1[CH:4]=[C:5]([C:8]2[CH:9]=[CH:10][C:11]3[S:17](=[O:18])(=[O:19])[CH2:16][CH2:15][C:14]([C:20]([OH:22])=[O:21])=[CH:13][C:12]=3[CH:24]=2)[S:6][CH:7]=1

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 21995692Methyl 7-(4-methyl-2-thienyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate

生成物 1

HCID 219958967-(4-Methyl-2-thienyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
100 °C

実験手順

In 1,2-dimethoxyethane (15.3 ml) was dissolved methyl 7-(4-methyl-2-thienyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate. (510 mg), and to the solution was added 6N hydrochloric acid (10.2 ml). The mixture was stirred at 100° C. for 15 hours and cooled to room temperature. Under reduced pressure, the solvent was evaporated. To the residue,were added ethyl acetate and potassium carbonate solution, and the mixture was extracted with water. To the solution was added 6N hydrochloric acid, and the solution was made pH 4-5, extracted with ethyl acetate, washed with saturated brine and dried with magnesium sulfate. Under reduced pressure, the solvent was evaporated to give 7-(4-methyl-2-thienyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (459 mg).

後処理

  1. temperaturecooled to room temperature
  2. customUnder reduced pressure, the solvent was evaporated
  3. additionTo the residue,were added ethyl acetate and potassium carbonate solution
  4. extractionthe mixture was extracted with water
  5. additionTo the solution was added 6N hydrochloric acid
  6. extractionextracted with ethyl acetate
  7. washwashed with saturated brine
  8. dry with materialdried with magnesium sulfate
  9. customUnder reduced pressure, the solvent was evaporated

出典と根拠

ORDレコード
ord-b8f8600acfff448da21d8681cfb3191d
出典データセット
uspto-grants-2001_05
特許番号
US06235771B1

反応ノート

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