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

HRID 1498906
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HRID 1498906 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 4

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

생성물 1

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

시약·촉매·용매 2

HCID 6212Chloroform
용매
HCID 8028Tetrahydrofuran용매2회

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온도
0 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8d9a8dc1f44042208113ba2f3fba5115
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09200008B2

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