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Lithium Hydroxide → HCID 22063596, 화합물

HRID 1828472
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HRID 1828472 반응식
[CH3:1][O:2][C:3]1[CH:20]=[CH:19][C:6]([CH2:7][N:8]2[N:12]=[N:11][C:10]([CH2:13][C:14]([O:16]CC)=[O:15])=[N:9]2)=[CH:5][CH:4]=1.[OH-].[Li+]>O1CCCC1.CO.O>[CH3:1][O:2][C:3]1[CH:20]=[CH:19][C:6]([CH2:7][N:8]2[N:12]=[N:11][C:10]([CH2:13][C:14]([OH:16])=[O:15])=[N:9]2)=[CH:5][CH:4]=1
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참가 물질

5

반응물 2

HCID 3939Lithium HydroxideHCID 15090418HCID 15090418, 화합물2회

생성물 1

HCID 22063596HCID 22063596, 화합물수율 98.9%

시약·촉매·용매 2

HCID 962Water용매HCID 21899815MeOH tetrahydrofuran용매

실험 절차

The ethyl 2-[2-(4-methoxybenzyl)-2H-1,2,3,4-tetrazol-5-yl]acetate (2.15 g, 7.78 mmol) obtained in (A) was dissolved in tetrahydrofuran/methanol (3:1, v/v, 60 ml), added dropwise with a solution of lithium hydroxide (359.2 mg, 8.56 mmol) in water (15 ml) under ice cooling and then stirred at room temperature for 2 hours. The solvent was evaporated, and the residue was added with 1 N aqueous hydrochloric acid to obtain pH of about 1. The solution was extracted with ethyl acetate, and the organic layer was washed with saturated brine and dried over anhydrous sodium sulfate. Then, the solvent was evaporated to obtain the title compound (1.91 g, 98.8%).

후처리

  1. customThe solvent was evaporated
  2. additionthe residue was added with 1 N aqueous hydrochloric acid
  3. customto obtain pH of about 1
  4. extractionThe solution was extracted with ethyl acetate
  5. washthe organic layer was washed with saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThen, the solvent was evaporated

출처 및 근거

ORD 기록
ord-25ab4b53c8204a019373176ac6b07ac3
출처 데이터셋
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07056917B2

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