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Hydrochloric Acid → HCID 59484992, 화합물

HRID 1850520
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인쇄 미리보기

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HRID 1850520 반응식
CO[C:3]1[CH:8]=[CH:7][C:6]([N:9]2[CH2:14][CH2:13][N:12]([C:15]3[C:16]([CH3:30])=[C:17]([CH3:29])[C:18]4[O:22][C:21]([CH2:24]C#N)([CH3:23])[CH2:20][C:19]=4[C:27]=3[CH3:28])[CH2:11][CH2:10]2)=[CH:5][CH:4]=1.[OH-:31].[Na+].[CH2:33](O)C.Cl.[C:37]([O:40]CC)(=[O:39])C>O>[CH3:33][O:31][C:3]1[CH:4]=[CH:5][C:6]([N:9]2[CH2:10][CH2:11][N:12]([C:15]3[C:16]([CH3:30])=[C:17]([CH3:29])[C:18]4[O:22][C:21]([CH2:24][C:37]([OH:40])=[O:39])([CH3:23])[CH2:20][C:19]=4[C:27]=3[CH3:28])[CH2:13][CH2:14]2)=[CH:7][CH:8]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 702EthanolHCID 8857Ethyl AcetateHCID 14798Sodium HydroxideHCID 59485094HCID 59485094, 화합물

생성물 1

HCID 59484992HCID 59484992, 화합물수율 55%

시약·촉매·용매 1

HCID 962
Water
용매

실험 절차

A mixture of {5-[4-(4-methoxyphenyl)piperazin-1-yl]-2,4,6,7-tetramethyl-2,3-dihydro-1-benzofuran-2-yl}acetonitrile (260 mg, 0.641 mmol) synthesized in Example 140, 8N sodium hydroxide aqueous solution (2.0 mL) and ethanol (10 mL) was stirred under heated reflux for 15 hours. After cooled to room temperature, 1N hydrochloric acid (16 mL) was added thereto, and the reaction solution was distributed using water and ethyl acetate. The organic layer was washed with saturated saline and dried using anhydrous magnesium sulfate, and then the solvent was removed under reduced pressure. The obtained residue was purified by silica gel chromatography (hexane-ethyl acetate 90:10-70:30) and crystallized from ethyl acetate-hexane to obtain 150 mg of the title compound (yield 55%). Melting point was 171 to 174° C. (decomposition).

후처리

  1. temperatureunder heated
  2. temperaturereflux for 15 hours
  3. washThe organic layer was washed with saturated saline
  4. customdried
  5. customthe solvent was removed under reduced pressure
  6. customThe obtained residue was purified by silica gel chromatography (hexane-ethyl acetate 90:10-70:30)
  7. customcrystallized from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-ec4b74d2a89a4198a06ae22d1c436a22
출처 데이터셋
uspto-grants-2015_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08957069B2

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