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Lithium hydroxide, monohydrate → 4-((E)-2-tert-Butoxycarbonyl-vinyl)-3-methyl-benzoic Acid

HRID 220862
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HRID 220862 반응식
O.[OH-].[Li+].C[O:5][C:6](=[O:23])[C:7]1[CH:12]=[CH:11][C:10](/[CH:13]=[CH:14]/[C:15]([O:17][C:18]([CH3:21])([CH3:20])[CH3:19])=[O:16])=[C:9]([CH3:22])[CH:8]=1>C1COCC1.O>[C:18]([O:17][C:15](/[CH:14]=[CH:13]/[C:10]1[CH:11]=[CH:12][C:7]([C:6]([OH:23])=[O:5])=[CH:8][C:9]=1[CH3:22])=[O:16])([CH3:21])([CH3:20])[CH3:19]
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참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 575553844-((E)-2-tert-Butoxycarbonyl-vinyl)-3-methyl-benzoic Acid Methyl Ester

생성물 1

HCID 575553374-((E)-2-tert-Butoxycarbonyl-vinyl)-3-methyl-benzoic Acid수율 92%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

Lithium hydroxide monohydrate (384 mg, 9.2 mmol) was added to a solution of 4-((E)-2-tert-butoxycarbonyl-vinyl)-3-methyl-benzoic acid methyl ester from Example E30.1 (1.27 g, 4.6 mmol) in THF (50 ml) and water (20 ml). The mixture was stirred for 20 h at room temperature then solvents were removed in vacuo. The residue was dissolved in EtOAc, washed with 1M KHSO4, water then brine, dried and concentrated in vacuo to yield the title compound (1.1 g, 92%).

후처리

  1. customsolvents were removed in vacuo
  2. dissolutionThe residue was dissolved in EtOAc
  3. washwashed with 1M KHSO4, water
  4. dry with materialbrine, dried
  5. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-448e9afca7f04cdf80f5039883741757
출처 데이터셋
uspto-grants-2012_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08202858B2

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