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

HRID 350227ノート

反応式

HRID 350227 の反応式
[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

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8028TetrahydrofuranHCID 14798Sodium HydroxideHCID 69423995HCID 69423995、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-94f18fd0b671472892d93ef5d2641ca4
出典データセット
uspto-grants-2007_02
特許番号
US07179823B1

反応ノート

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