Potassium Hydroxide → 2-(Hydroxymethyl)-5-methylbenzoic acid

HRID 2361332

反応式

HRID 2361332 の反応式
[CH3:1][C:2]1[CH:10]=[C:9]2[C:5]([CH2:6][O:7][C:8]2=[O:11])=[CH:4][CH:3]=1.[OH-:12].[K+]>CO.O>[OH:12][CH2:6][C:5]1[CH:4]=[CH:3][C:2]([CH3:1])=[CH:10][C:9]=1[C:8]([OH:7])=[O:11]

参加物

5

反応物 2

HCID 14797Potassium HydroxideHCID 6387566-Methylphthalide

生成物 1

HCID 679628172-(Hydroxymethyl)-5-methylbenzoic acid収率 59.4%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

A colorless, homogeneous solution of 6-methylisobenzofuran-1(3H)-one (0.95 g, 6.41 mmol), KOH (0.576 g, 10.26 mmol) in methanol (20.52 mL) and water (5.13 mL) was refluxed. After two hr, the reaction was cooled to room temperature, concentrated in vacuo, and acidified with 1 M aqueous KHSO4 to pH ˜3. The mixture was extracted with EtOAc (4×50 mL). The combined extract was dried over MgSO4 and concentrated in vacuo to give the desired product (0.632 g, 3.81 mmol, 59.4% yield) as a white solid.

後処理

  1. concentrationconcentrated in vacuo
  2. extractionThe mixture was extracted with EtOAc (4×50 mL)
  3. extractionThe combined extract
  4. dry with materialwas dried over MgSO4
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-8707a0efd23f4914ba4fe44be75131be
出典データセット
uspto-grants-2014_04
特許番号
US08685969B2

関連ノート

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