Dimethylformamide → Methyl 5-acetyl-2-methoxybenzoate

HRID 218350

반응식

HRID 218350 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

HCID 606426Methyl 5-acetyl-2-methoxybenzoate

시약·촉매·용매 1

HCID 962Water용매3회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-cc464edf098343589f6ec4a3f468f497
출처 데이터셋
uspto-grants-2012_06
특허 번호
US08198441B2

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