Potassium Carbonate → Methyl 4-(3-chloropropoxy)-3-methoxybenzoate

HRID 612027

反応式

HRID 612027 の反応式
C1(C)C=CC(S(O[CH2:11][CH2:12][CH2:13][Cl:14])(=O)=O)=CC=1.[CH3:16][O:17][C:18](=[O:28])[C:19]1[CH:24]=[C:23]([O:25][CH3:26])[C:22]([OH:27])=[CH:21][CH:20]=1.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH3:16][O:17][C:18](=[O:28])[C:19]1[CH:24]=[C:23]([O:25][CH3:26])[C:22]([O:27][CH2:11][CH2:12][CH2:13][Cl:14])=[CH:21][CH:20]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 19844Methyl VanillateHCID 694343-Chloropropyl p-toluenesulfonate

生成物 1

HCID 14407173Methyl 4-(3-chloropropoxy)-3-methoxybenzoate収率 99.5%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

A mixture of 102.4 g (411.7 mmol) of 3-chloropropyl p-toluene sulfonate, 75 g (411.7 mmol) of 4-hydroxy-5-methoxy -benzoic acid methyl ester, 75.7 g (547.5 mmol) of potassium carbonate, and 1.66 g (4.1 mmol) of methyl-tricapryl ammonium chloride in 900 ml of acetone was stirred rapidly at reflux for 18 hr. The mixture was filtered and the solvent was removed giving 106 g of the tile compound after recrystallization from a chloroform-hexane mixture.

後処理

  1. temperatureat reflux for 18 hr
  2. filtrationThe mixture was filtered
  3. customthe solvent was removed

出典と根拠

ORDレコード
ord-c8f2827ba64e489d8f06f816ca2b60ff
出典データセット
uspto-grants-1999_12
特許番号
US06002008

関連ノート

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