Chloroform → Ethyl 2-(4-methoxyphenyl)-2-oxoacetate

HRID 1859305ノート

反応式

HRID 1859305 の反応式
[Cl-].[Al+3].[Cl-].[Cl-].C(Cl)(Cl)Cl.[CH2:9]([O:11][C:12](=[O:16])[C:13](Cl)=[O:14])[CH3:10].[C:17]1([O:23][CH3:24])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>O>[CH2:9]([O:11][C:12](=[O:16])[C:13]([C:20]1[CH:21]=[CH:22][C:17]([O:23][CH3:24])=[CH:18][CH:19]=1)=[O:14])[CH3:10]

参加物

6

反応物 4

HCID 6212ChloroformHCID 7519AnisoleHCID 20884Ethoxalyl chlorideHCID 6451240Aluminum(III) Chloride

生成物 1

HCID 2758864Ethyl 2-(4-methoxyphenyl)-2-oxoacetate

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
5 °C

実験手順

Aluminum chloride (84.30 g, 632 mmol) was added to chloroform (300 ml) and chloroglyoxylic ethyl ester (60 g, 439 mmol) was added dropwise to the resulting suspension over 20 minutes at 0° C. The reaction mixture was stirred for 40 minutes at 5° C. At the same temperature, anisole (68.79 g, 636 mmol) was slowly added dropwise to the reaction solution and then stirred for 12 hours at 10° C. When the reaction is completed, the reaction solution was cooled and, after adding cooling water (100 ml), extracted with dichloromethane. The extract was dried over anhydrous magnesium sulfate and then concentrated to obtain the title compound as a yellow solid (TLC identification). The resulting compound was used in the next reaction without further purification.

後処理

  1. additionwas added dropwise to the resulting suspension over 20 minutes at 0° C
  2. stirringstirred for 12 hours at 10° C
  3. temperaturethe reaction solution was cooled
  4. additionafter adding
  5. extractionextracted with dichloromethane
  6. dry with materialThe extract was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-51cd687d5e5945039a67b12a8cd3f9ea
出典データセット
uspto-grants-2000_11
特許番号
US06153768

反応ノート

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