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Lithium hydroxide, monohydrate → 2-tert-Butoxy-5-methanesulfonyl-benzoic acid

HRID 2251182
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HRID 2251182 반응식
C[O:2][C:3](=[O:19])[C:4]1[CH:9]=[C:8]([S:10]([CH3:13])(=[O:12])=[O:11])[CH:7]=[CH:6][C:5]=1[O:14][C:15]([CH3:18])([CH3:17])[CH3:16].O.[OH-].[Li+]>C1COCC1.O>[C:15]([O:14][C:5]1[CH:6]=[CH:7][C:8]([S:10]([CH3:13])(=[O:12])=[O:11])=[CH:9][C:4]=1[C:3]([OH:19])=[O:2])([CH3:18])([CH3:17])[CH3:16]
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참가 물질

5

반응물 2

HCID 168937Lithium hydroxide, monohydrateHCID 586778292-tert-Butoxy-5-methanesulfonyl-benzoic acid methyl ester

생성물 1

HCID 211002592-tert-Butoxy-5-methanesulfonyl-benzoic acid수율 66.6%

시약·촉매·용매 2

HCID 962Water용매HCID 8028Tetrahydrofuran용매

실험 절차

To 2-tert-Butoxy-5-methanesulfonyl-benzoic acid methyl ester (1.58 g) in THF (25 mL) was added a solution lithium hydroxide monohydrate (0.35 g) in water (25 mL), and the reaction mixture was stirred at room temperature for 4 hours. After such time, the THF was removed in vacuo and to the remaining aqueous solution was added 8 mL of 1N HCl solution, leading to precipitation of the compound. The precipitate was filtered off and washed several times with water to yield the title compound (1.00 g) as a white solid. MS (m/e): 289.9 (M+NH4+).

후처리

  1. customAfter such time, the THF was removed in vacuo and to the remaining aqueous solution
  2. additionwas added 8 mL of 1N HCl solution
  3. customleading to precipitation of the compound
  4. filtrationThe precipitate was filtered off
  5. washwashed several times with water

출처 및 근거

ORD 기록
ord-62654bdf93d741c78cd9cda1b95bd05e
출처 데이터셋
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07319099B2

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