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Hydrochloric Acid → Ethyl 4-(2,4-dichlorophenyl)-2,4-dioxobutanoate

HRID 1498906
ノート
印刷プレビュー

反応式

HRID 1498906 の反応式
[O-]CC.[Na+].C(O)C.[Cl:8][C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:10]=1[C:16](=[O:18])[CH3:17].[C:19](OCC)(=[O:25])[C:20]([O:22][CH2:23][CH3:24])=[O:21].Cl>O1CCCC1.C(Cl)(Cl)Cl>[Cl:8][C:9]1[CH:14]=[C:13]([Cl:15])[CH:12]=[CH:11][C:10]=1[C:16](=[O:18])[CH2:17][C:19](=[O:25])[C:20]([O:22][CH2:23][CH3:24])=[O:21]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 7268Diethyl OxalateHCID 166932',4'-DichloroacetophenoneHCID 23706232Ethanol sodium ethoxide

生成物 1

HCID 22997478Ethyl 4-(2,4-dichlorophenyl)-2,4-dioxobutanoate収率 78.2%

試薬・触媒・溶媒 2

HCID 6212Chloroform溶媒
HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
0 °C

実験手順

A 20% sodium ethoxide-ethanol solution (17 g) was added to tetrahydrofuran (100 ml), and the mixture was cooled to 0° C. It took 60 minutes to dropwise add a solution of 2′,4′-dichloroacetophenone (9.45 g) and diethyl oxalate (7.30 g) in tetrahydrofuran (100 ml) to the mixture. After the completion of the dropping, the mixture was allowed to warm to a room temperature and stirred for 2 hours. To the mixture, 2-N hydrochloric acid (200 ml) and chloroform (200 ml) were added. The organic layer was collected by separation and dried over anhydrous magnesium sulfate, and the solvent was distilled off. Thus, the title compound (11.3 g, 78%) as a light-brown oily substance was obtained.

後処理

  1. temperatureto warm to a room temperature
  2. customThe organic layer was collected by separation
  3. dry with materialdried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off

出典と根拠

ORDレコード
ord-8d9a8dc1f44042208113ba2f3fba5115
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09200008B2

反応ノート

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