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Lithium Hydroxide → HCID 22063596、化合物

HRID 1828472
ノート
印刷プレビュー

反応式

HRID 1828472 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 3939Lithium HydroxideHCID 15090418HCID 15090418、化合物2 回

生成物 1

HCID 22063596HCID 22063596、化合物収率 98.9%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 21899815MeOH tetrahydrofuran溶媒

実験手順

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%).

後処理

  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

出典と根拠

ORDレコード
ord-25ab4b53c8204a019373176ac6b07ac3
出典データセット
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07056917B2

反応ノート

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