Hydrochloric Acid → 3-[1-[4-(2-Methyl-3-pyridylmethoxy)benzyl]-4-phenyl-3-pyrrolyl]propionic acid

HRID 350052

반응식

HRID 350052 반응식
[CH3:1][C:2]1[C:7]([CH2:8][O:9][C:10]2[CH:34]=[CH:33][C:13]([CH2:14][N:15]3[CH:19]=[C:18]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=4)[C:17]([CH2:26][CH2:27][C:28]([O:30]CC)=[O:29])=[CH:16]3)=[CH:12][CH:11]=2)=[CH:6][CH:5]=[CH:4][N:3]=1.[OH-].[Na+].O1CCCC1.Cl>C(O)C>[CH3:1][C:2]1[C:7]([CH2:8][O:9][C:10]2[CH:34]=[CH:33][C:13]([CH2:14][N:15]3[CH:19]=[C:18]([C:20]4[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=4)[C:17]([CH2:26][CH2:27][C:28]([OH:30])=[O:29])=[CH:16]3)=[CH:12][CH:11]=2)=[CH:6][CH:5]=[CH:4][N:3]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 69423888Ethyl 3-[1-[4-(2-methyl-3-pyridylmethoxy)benzyl]-4-phenyl-3-pyrrolyl]propionate

생성물 1

HCID 694229823-[1-[4-(2-Methyl-3-pyridylmethoxy)benzyl]-4-phenyl-3-pyrrolyl]propionic acid수율 87.3%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of ethyl 3-[1-[4-(2-methy-3-pyridylmethoxy)benzyl]-4-phenyl-3-pyrrolyl]propionate (568 mg), 1N aqueous sodium hydroxide solution (3 ml), tetrahydrofuran (6 ml), and ethanol (6 ml) was stirred at room temperature for 4 hours, and 1N hydrochloric acid (3 ml) was added to the mixture, which was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated aqueous sodium chloride solution, dried (MgSO4), then concentrated. The colorless crystals obtained were collected by filtration to yield 3-[1-[4-(2-methyl-3-pyridylmethoxy)benzyl]-4-phenyl-3-pyrrolyl]propionic acid (465 mg, yield: 87%). This was recrystallized from ethyl acetate-hexane. Melting point: 158–159° C.

후처리

  1. extractionwas extracted with ethyl acetate
  2. washThe ethyl acetate layer was washed with saturated aqueous sodium chloride solution
  3. dry with materialdried (MgSO4)
  4. concentrationconcentrated
  5. customThe colorless crystals obtained
  6. filtrationwere collected by filtration

출처 및 근거

ORD 기록
ord-a1d29a95cb484d83908bf18e6ebcce29
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07179823B1

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