Hydrochloric Acid → 7-(4-Methoxyphenyl)-2,3-dihydro-1-benzo-thiepine-4-carboxylic acid

HRID 2228265노트

반응식

HRID 2228265 반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:10]=[CH:11][C:12]3[S:18][CH2:17][CH2:16][C:15]([C:19]([O:21]C)=[O:20])=[CH:14][C:13]=3[CH:23]=2)=[CH:5][CH:4]=1.[OH-].[Na+].Cl>C(O)C.C1COCC1>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2[CH:10]=[CH:11][C:12]3[S:18][CH2:17][CH2:16][C:15]([C:19]([OH:21])=[O:20])=[CH:14][C:13]=3[CH:23]=2)=[CH:5][CH:4]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 18472336Methyl 7-(4-methoxyphenyl)-2,3-dihydro-1-benzothiepine-4-carboxylate

생성물 1

HCID 184723977-(4-Methoxyphenyl)-2,3-dihydro-1-benzo-thiepine-4-carboxylic acid수율 106.2%

시약·촉매·용매 1

HCID 21873804Tetrahydrofuran ethanol용매

실험 절차

To a solution of methyl 7-(4-methoxyphenyl)-2,3-dihydro-1-benzothiepine-4-carboxylate (0.50 g) in ethanol/THF (10/10 ml) was added at room temperature 1N sodium hydroxide solution (2 ml), and the mixture was stirred for 18 hours. To the mixture was added 1N hydrochloric acid (2 ml). Under reduced pressure, the mixture was concentrated. To the mixture was added water, and the precipitates were collected by filtration, which were washed with 2-propanol, diethylether and hexane to give pale yellow solid of 7-(4-methoxyphenyl)-2,3-dihydro-1-benzo-thiepine-4-carboxylic acid (508 mg). This compound was used for the following reaction, without subjecting further purification.

후처리

  1. concentrationUnder reduced pressure, the mixture was concentrated
  2. additionTo the mixture was added water
  3. filtrationthe precipitates were collected by filtration, which
  4. washwere washed with 2-propanol, diethylether and hexane

출처 및 근거

ORD 기록
ord-850d57be16814bfd8fb2f3521aa58da3
출처 데이터셋
uspto-grants-2002_07
특허 번호
US06413947B1

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