Methyl 7-(4-piperidinophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate → 7-(4-Piperidinophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid

HRID 1978587노트

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HRID 1978587 반응식
[N:1]1([C:7]2[CH:12]=[CH:11][C:10]([C:13]3[CH:14]=[CH:15][C:16]4[S:22](=[O:24])(=[O:23])[CH2:21][CH2:20][C:19]([C:25]([O:27]C)=[O:26])=[CH:18][C:17]=4[CH:29]=3)=[CH:9][CH:8]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1>Cl>[N:1]1([C:7]2[CH:12]=[CH:11][C:10]([C:13]3[CH:14]=[CH:15][C:16]4[S:22](=[O:24])(=[O:23])[CH2:21][CH2:20][C:19]([C:25]([OH:27])=[O:26])=[CH:18][C:17]=4[CH:29]=3)=[CH:9][CH:8]=2)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1

참가 물질

3

반응물 1

HCID 21995918Methyl 7-(4-piperidinophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate

생성물 1

HCID 219959647-(4-Piperidinophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid수율 94.8%

시약·촉매·용매 1

HCID 313Hydrochloric Acid용매

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온도
70 °C

실험 절차

To methyl 7-(4-piperidinophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate (600 mg) was added 6N hydrochloric acid (60 ml), and the mixture was stirred at 70° C. for 5 hours and concentrated under reduced pressure. To the residue was added ethanol, and to the mixture were added 8N sodium hydroxide solution and 1N sodium hydroxide solution to make the solution pH 6-7. The mixture was concentrated under reduced pressure to give solid, which was collected by filtration and washed with water, 2-propanol, acetone and diisopropylether to give yellow powder of 7-(4-piperidinophenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid (549.5 mg).

후처리

  1. concentrationconcentrated under reduced pressure
  2. additionTo the residue was added ethanol
  3. additionto the mixture were added 8N sodium hydroxide solution and 1N sodium hydroxide solution
  4. concentrationThe mixture was concentrated under reduced pressure
  5. customto give solid, which
  6. filtrationwas collected by filtration
  7. washwashed with water, 2-propanol, acetone and diisopropylether

출처 및 근거

ORD 기록
ord-1c0ad464721b4e82a06b1f16ea7a3fe0
출처 데이터셋
uspto-grants-2001_05
특허 번호
US06235771B1

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