Hydrochloric Acid → Ethyl 6-(4-chlorophenyl)-2,4,6-trioxohexanoate

HRID 544170

反応式

HRID 544170 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=[O:13])[CH2:9][C:10](=[O:12])[CH3:11])=[CH:4][CH:3]=1.[C:14](OCC)(=[O:20])[C:15]([O:17][CH2:18][CH3:19])=[O:16].[H-].[Na+].Cl>COCCOC>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]([C:8](=[O:13])[CH2:9][C:10](=[O:12])[CH2:11][C:14](=[O:20])[C:15]([O:17][CH2:18][CH3:19])=[O:16])=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7268Diethyl OxalateHCID 24758Sodium hydrideHCID 2380831-(4-Chlorophenyl)butane-1,3-dione

生成物 1

HCID 15578432Ethyl 6-(4-chlorophenyl)-2,4,6-trioxohexanoate

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒2 回

実験手順

A solution of 1-(4-chlorophenyl)-1,3-butanedione (0.6 g) and diethyl oxalate (0.83 ml) in 1,2-dimethoxyethane (2 ml) was added to a stirred suspension of sodium hydride (0.44 g, 50% dispersion in mineral oil, washed with petrol 40°-60° C.) in 1,2-dimethoxyethane (5 ml) under nitrogen. The stirred mixture was heated under reflux for 1 hour, cooled and acidified with 2M hydrochloric acid (10 ml). The brown solid which formed was recrystallised from ethanol-water to give the title product (mp 93°-94° C.).

後処理

  1. temperatureThe stirred mixture was heated
  2. temperatureunder reflux for 1 hour
  3. temperaturecooled
  4. customThe brown solid which formed
  5. customwas recrystallised from ethanol-water

出典と根拠

ORDレコード
ord-d64d2eb4bba64c0b8da63df92b365699
出典データセット
uspto-grants-1984_05
特許番号
US04448787

関連ノート

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