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

HRID 413596노트

반응식

HRID 413596 반응식
[CH2:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:12]=[CH:13][C:14]3[S:20](=[O:22])(=[O:21])[CH2:19][CH2:18][C:17]([C:23]([O:25]CC)=[O:24])=[CH:16][C:15]=3[CH:28]=2)=[CH:7][CH:6]=1)[CH2:2][CH3:3].C(=O)([O-])[O-].[K+].[K+].Cl>O1CCCC1.CO.O>[CH2:1]([O:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:12]=[CH:13][C:14]3[S:20](=[O:21])(=[O:22])[CH2:19][CH2:18][C:17]([C:23]([OH:25])=[O:24])=[CH:16][C:15]=3[CH:28]=2)=[CH:7][CH:6]=1)[CH2:2][CH3:3]

참가 물질

7

반응물 3

HCID 313Hydrochloric Acid2회HCID 11430Potassium CarbonateHCID 11773971Ethyl 7-(4-propoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylate

생성물 1

HCID 111646457-(4-Propoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid수율 96%

시약·촉매·용매 3

HCID 887Methanol용매HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

Ethyl 7-(4-propoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxlate (495 g, 1.24 mol) was dissolved in 4.95 L of tetrahydrofuran and 2.48 L of methanol. Crystals were formed by adding a potassium carbonate (342 g, 2.47 mol) solution in 4.2 L of water and the mixture was heated under reflux for 6.5 hours. Under reflux, 1.85 L of a 3N hydrochloric acid was dropped to form crystals. After cooling, 84 ml of a 6N hydrochloric acid was added at room temperature (pH 2-3) and stirred for 1 hour while cooling in ice. After filtration, the residue was washed with 2.97 L of a mixed solution of tetrahydrofuran/methanol/water=1/1/3 . After vacuum drying (40° C.), 443 g (Yield 96%) of 7-(4-propoxyphenyl)-1,1-dioxo-2,3-dihydro-1-benzothiepine-4-carboxylic acid was obtained as pale yellowish white crystals.

후처리

  1. customCrystals were formed
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 6.5 hours
  4. temperatureUnder reflux
  5. customto form crystals
  6. temperatureAfter cooling
  7. temperaturewhile cooling in ice
  8. filtrationAfter filtration
  9. washthe residue was washed with 2.97 L of a mixed solution of tetrahydrofuran/methanol/water=1/1/3
  10. customAfter vacuum drying (40° C.)

출처 및 근거

ORD 기록
ord-ae4946f98d5540029bb495c7d0ce904b
출처 데이터셋
uspto-grants-2003_05
특허 번호
US06566535B1

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