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Acetic Anhydride → 2-Methyl-6-acetamidobenzyl alcohol

HRID 2073795
ノート
印刷プレビュー

反応式

HRID 2073795 の反応式
[NH2:1][C:2]1[CH:9]=[CH:8][CH:7]=[C:6]([CH3:10])[C:3]=1[CH2:4][OH:5].[C:11](OC(=O)C)(=[O:13])[CH3:12].C(=O)(O)[O-].[Na+]>C(Cl)Cl>[CH3:10][C:6]1[CH:7]=[CH:8][CH:9]=[C:2]([NH:1][C:11](=[O:13])[CH3:12])[C:3]=1[CH2:4][OH:5]
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 3

HCID 7918Acetic AnhydrideHCID 516892Sodium BicarbonateHCID 15339417(2-Amino-6-methylphenyl)methanol

生成物 1

HCID 143684642-Methyl-6-acetamidobenzyl alcohol収率 64.6%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a suspension of 2-amino-6-methylbenzyl alcohol (30 g) in methylene chloride (300 ml) was added dropwise acetic anhydride (22.3 g) at 5° to 10° C. After being stirred for 3 hours, the mixture was neutralized with sodium bicarbonate aqueous solution to give precipitates. To said mixture was added chloroform to dissolve said precipitates and then the organic layer was washed with water and sodium chloride aqueous solution, dried over magnesium sulfate and evaporated in vacuo. The resultant residue was suspended in diethyl ether and the precipitates were collected by filtration to give 2-methyl-6-acetamidobenzyl alcohol (25.30 g).

後処理

  1. customto give
  2. customprecipitates
  3. additionwas added chloroform
  4. dissolutionto dissolve
  5. customsaid precipitates
  6. washthe organic layer was washed with water and sodium chloride aqueous solution
  7. dry with materialdried over magnesium sulfate
  8. customevaporated in vacuo
  9. filtrationthe precipitates were collected by filtration

出典と根拠

ORDレコード
ord-a80899f975f149b7b0505acf426b856d
出典データセット
uspto-grants-1990_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04920129

反応ノート

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