Sodium Hydroxide → 3-Methyl-2-(2-methyl-1-propenyl)benzoic acid

HRID 1047902ノート

反応式

HRID 1047902 の反応式
C([O:3][C:4](=[O:16])[C:5]1[CH:10]=[CH:9][CH:8]=[C:7]([CH3:11])[C:6]=1[CH:12]=[C:13]([CH3:15])[CH3:14])C.[OH-].[Na+]>CO>[CH3:11][C:7]1[C:6]([CH:12]=[C:13]([CH3:15])[CH3:14])=[C:5]([CH:10]=[CH:9][CH:8]=1)[C:4]([OH:16])=[O:3]

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 59314297HCID 59314297、化合物

生成物 1

HCID 593140863-Methyl-2-(2-methyl-1-propenyl)benzoic acid収率 75%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of the 3-methyl-2-(2-methyl-1-propenyl)benzoic acid ethyl ester (290) (3 g-0.014 mol) in MeOH (50 mL) is treated with 2N NaOH (10 mL) and refluxed for 6 h. The solvent is removed in vacuo and the residue diluted with water (75 mL). The aqueous phase is extracted with EtOAc (30 mL) and then separated and acidified to pH 2-3 with concentrated HCl. The solid precipitated is extracted into EtOAc (3×50 mL). The extracts are washed with water (2×30 mL) and brine (2×30 mL), and dried over MgSO4 and concentrated in vacuo to give the product as white solid (2.0 g, 75%).

後処理

  1. temperaturerefluxed for 6 h
  2. customThe solvent is removed in vacuo
  3. additionthe residue diluted with water (75 mL)
  4. extractionThe aqueous phase is extracted with EtOAc (30 mL)
  5. customseparated
  6. customThe solid precipitated
  7. extractionis extracted into EtOAc (3×50 mL)
  8. washThe extracts are washed with water (2×30 mL) and brine (2×30 mL)
  9. dry with materialdried over MgSO4
  10. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-78c7b5d3225e448e96513667760356eb
出典データセット
uspto-grants-2013_10
特許番号
US08569535B2

反応ノート

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