Hydrochloric Acid → 3-[1-[4-(1H-benzotriazol-1-ylmethoxy)benzyl]-3-ethoxy-1H-pyrazol-4-yl]propionic acid

HRID 350227노트

반응식

HRID 350227 반응식
[N:1]1([CH2:10][O:11][C:12]2[CH:33]=[CH:32][C:15]([CH2:16][N:17]3[CH:21]=[C:20]([CH2:22][CH2:23][C:24]([O:26]CC)=[O:25])[C:19]([O:29][CH2:30][CH3:31])=[N:18]3)=[CH:14][CH:13]=2)[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[N:2]1.[OH-].[Na+].O1CCCC1.Cl>C(O)C>[N:1]1([CH2:10][O:11][C:12]2[CH:13]=[CH:14][C:15]([CH2:16][N:17]3[CH:21]=[C:20]([CH2:22][CH2:23][C:24]([OH:26])=[O:25])[C:19]([O:29][CH2:30][CH3:31])=[N:18]3)=[CH:32][CH:33]=2)[C:5]2[CH:6]=[CH:7][CH:8]=[CH:9][C:4]=2[N:3]=[N:2]1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 69423995HCID 69423995, 화합물

생성물 1

HCID 694245383-[1-[4-(1H-benzotriazol-1-ylmethoxy)benzyl]-3-ethoxy-1H-pyrazol-4-yl]propionic acid수율 94.2%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

After a mixture of ethyl 3-[1-[4-(1H-benzotriazol-1-ylmethoxy)benzyl]-3-ethoxy-1H-pyrazol-4-yl]propionate (652 mg), 1N aqueous sodium hydroxide solution (3 ml), tetrahydrofuran (6 ml) and ethanol (6 ml) was stirred at room temperature for 3 hours, 1N hydrochloric acid (3 ml) was added to the mixture, and then 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-[1-[4-(1H-benzotriazol-1-ylmethoxy)benzyl]-3-ethoxy-1H-pyrazol-4-yl]propionic acid (576 mg, yield: 94%). This was recrystallized from ethanol-hexane. Melting point: 136–137° 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-94f18fd0b671472892d93ef5d2641ca4
출처 데이터셋
uspto-grants-2007_02
특허 번호
US07179823B1

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