Hydrochloric Acid → [3-phenyl-1-[6-(2-phenyl-4-thiazolylmethoxy)-3-pyridylmethyl]-1H-pyrazol-4-yl]acetic acid

HRID 350297노트

반응식

HRID 350297 반응식
[C:1]1([C:7]2[C:11]([CH2:12][C:13]([O:15]CC)=[O:14])=[CH:10][N:9]([CH2:18][C:19]3[CH:20]=[N:21][C:22]([O:25][CH2:26][C:27]4[N:28]=[C:29]([C:32]5[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=5)[S:30][CH:31]=4)=[CH:23][CH:24]=3)[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[OH-].[Na+].O1CCCC1.Cl>C(O)C>[C:1]1([C:7]2[C:11]([CH2:12][C:13]([OH:15])=[O:14])=[CH:10][N:9]([CH2:18][C:19]3[CH:20]=[N:21][C:22]([O:25][CH2:26][C:27]4[N:28]=[C:29]([C:32]5[CH:37]=[CH:36][CH:35]=[CH:34][CH:33]=5)[S:30][CH:31]=4)=[CH:23][CH:24]=3)[N:8]=2)[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 86760433ethyl [3-phenyl-1-(6-(2-phenyl-4-thiazolylmethoxy)-3-pyridylmethyl]-1H-pyrazol-4-yl]acetate

생성물 1

HCID 69422951[3-phenyl-1-[6-(2-phenyl-4-thiazolylmethoxy)-3-pyridylmethyl]-1H-pyrazol-4-yl]acetic acid수율 91%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

After a mixture of ethyl [3-phenyl-1-(6-(2-phenyl-4-thiazolylmethoxy)-3-pyridylmethyl]-1H-pyrazol-4-yl]acetate (536 mg), 1N sodium hydroxide solution (2 ml), tetrahydrofuran (4 ml), and ethanol (4 ml) was stirred at room temperature for 2 hours, 1N hydrochloric acid (2 ml) was added to the mixture, and the mixture was extracted with ethyl acetate. The ethyl acetate layer was washed with saturated aqueous sodium chloride solution, dried (MgSO4), and concentrated. The resulting colorless crystals were collected by filtration to obtain [3-phenyl-1-[6-(2-phenyl-4-thiazolylmethoxy)-3-pyridylmethyl]-1H-pyrazol-4-yl]acetic acid (459 mg, yield: 91%). This was recrystallized from ethanol-hexane. Melting point: 118–119° C.

후처리

  1. extractionthe mixture was 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. filtrationThe resulting colorless crystals were collected by filtration

출처 및 근거

ORD 기록
ord-65b59db8415e49a5b3108ebee55f53ac
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07179823B1

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