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Water → Acetic acid, 5-methoxy-m-tolyl-

HRID 1833267
ノート
印刷プレビュー

反応式

HRID 1833267 の反応式
[C:1]([CH2:3][C:4]1[CH:9]=[C:8]([CH3:10])[CH:7]=[C:6]([O:11][CH3:12])[CH:5]=1)#N.[OH-:13].[Na+].[OH2:15]>C(O)C>[CH3:12][O:11][C:6]1[CH:5]=[C:4]([CH2:3][C:1]([OH:15])=[O:13])[CH:9]=[C:8]([CH3:10])[CH:7]=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 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 22048241(3-Methoxy-5-methylphenyl)acetonitrile

生成物 1

HCID 39879Acetic acid, 5-methoxy-m-tolyl-収率 62%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 1-bromomethyl-3-methoxy-5-methyl-benzene (1.66 g, 7.7 mmol) and sodium cyanide (1.89 g, 38.5 mmol) in ethanol (15 mL) and water (5 mL) was warmed to 60° C. for 2 hrs. The reaction mixture was cooled, concentrated in vacuo, diluted with water (100 mL), and extracted with methylene chloride (3×20 mL). The combined organic layers were dried over magnesium sulfate, filtered and concentrated in vacuo to afford 1.16 g of a light yellow oil. The crude 1-cyanomethyl-3-methoxy-5-methyl-benzene (1.16 g, 7.1 mmol) and sodium hydroxide (1.44 g, 35.9 mmol) in ethanol (20 mL) and water (10 mL) was refluxed overnight. The reaction mixture was cooled, concentrated in vacuo, diluted with water, and extracted with methylene chloride (3×10 mL). The aqueous layer was acidified to pH 2 with 6N hydrochloric acid and extracted with methylene chloride (3×20 mL). The combined organic layers were dried over magnesium sulfate, filtered and concentrated in vacuo to afford 0.86 g (62% for 2 steps) of (3-methoxy-5-methyl-phenyl)-acetic acid as an off white solid. This material was used without further purification: 1H NMR (300 MHz) compatible.

後処理

  1. temperatureThe reaction mixture was cooled
  2. concentrationconcentrated in vacuo
  3. additiondiluted with water
  4. extractionextracted with methylene chloride (3×10 mL)
  5. extractionextracted with methylene chloride (3×20 mL)
  6. dry with materialThe combined organic layers were dried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-f2f99fe4585548a08fcfe640e99a4521
出典データセット
uspto-grants-2006_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07067529B2

反応ノート

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