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Water → Ethyl 5-hydroxy-2-(5-methyltetrazol-1-yl)benzoate

HRID 598334
ノート
印刷プレビュー

反応式

HRID 598334 の反応式
C([O:4][C:5]1[CH:6]=[CH:7][C:8]([N:16]2[C:20]([CH3:21])=[N:19][N:18]=[N:17]2)=[C:9]([CH:15]=1)[C:10]([O:12][CH2:13][CH3:14])=[O:11])(=O)C.[O-]CC.[K+].O.[Cl-].[NH4+]>CN(C=O)C>[OH:4][C:5]1[CH:6]=[CH:7][C:8]([N:16]2[C:20]([CH3:21])=[N:19][N:18]=[N:17]2)=[C:9]([CH:15]=1)[C:10]([O:12][CH2:13][CH3:14])=[O:11]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 25517Ammonium ChlorideHCID 23670592Potassium ethoxideHCID 67051123Ethyl 5-acetoxy-2-(5-methyltetrazol-1-yl)benzoate

生成物 1

HCID 67050952Ethyl 5-hydroxy-2-(5-methyltetrazol-1-yl)benzoate収率 70.2%

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

Ethyl 5-acetoxy-2-(5-methyltetrazol-1-yl)benzoate (164 g, 0.565 mol) was dissolved in 500 mL of DMF and immersed in a water bath. Potassium ethoxide (52.3 g, 0.621 mol) was added to this solution portionwise, keeping the reaction temperature below 40° C. After 30 minutes, the reaction was poured into 4 L of water and ammonium chloride was added to the solution until the product precipitated. After one hour of stirring, the precipitate was filtered and dried under a flow of air to give 98.5 g of ethyl 5-hydroxy-2-(5-methyltetrazol-1-yl)benzoate as a white solid.

後処理

  1. customimmersed in a water bath
  2. customthe reaction temperature below 40° C
  3. additionwas added to the solution until the product
  4. customprecipitated
  5. filtrationthe precipitate was filtered
  6. customdried under a flow of air

出典と根拠

ORDレコード
ord-97e86591e9884432a6d069c582a8a2c3
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07897597B2

反応ノート

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