Dimethylformamide → Methyl 5-acetyl-2-methoxybenzoate

HRID 218350

反応式

HRID 218350 の反応式
[C:1]([C:4]1[CH:5]=[CH:6][C:7]([OH:14])=[C:8]([CH:13]=1)[C:9]([O:11][CH3:12])=[O:10])(=[O:3])[CH3:2].[CH3:15]N(C=O)C.C(=O)([O-])[O-].[K+].[K+].CI>O>[C:1]([C:4]1[CH:5]=[CH:6][C:7]([O:14][CH3:15])=[C:8]([CH:13]=1)[C:9]([O:11][CH3:12])=[O:10])(=[O:3])[CH3:2]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 6328Methyl iodideHCID 11430Potassium CarbonateHCID 85444Methyl 5-acetylsalicylate

生成物 1

HCID 606426Methyl 5-acetyl-2-methoxybenzoate

試薬・触媒・溶媒 1

HCID 962Water溶媒3 回

実験手順

Methyl 5-acetyl-2-hydroxybenzoate (95.3 g, 490.6 mmol) was added to DMF (381 mL) and potassium carbonate (82.2 g, 588.8 mmol) at RT under an atmosphere of nitrogen. To the resulting suspension was added methyl iodide (90.5 g, 637.8 mmol) whilst maintaining good agitation. After stirring at RT for 30 minutes, the crude reaction mixture was analysed by GC demonstrating complete reaction. Water (380 mL) was added followed by further water (380 mL) and the resulting white solid filtered off to afford 82.5 g of the desired, water wet product (7).

後処理

  1. temperaturewhilst maintaining good agitation
  2. customthe crude reaction mixture
  3. customwas analysed by GC demonstrating complete reaction
  4. filtrationthe resulting white solid filtered off
  5. customto afford 82.5 g of the

出典と根拠

ORDレコード
ord-cc464edf098343589f6ec4a3f468f497
出典データセット
uspto-grants-2012_06
特許番号
US08198441B2

関連ノート

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