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Hydrochloric Acid → Methyl 4-(2-chlorophenyl)-2,4-dioxobutanoate

HRID 1498930
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인쇄 미리보기

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HRID 1498930 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[O:10])[CH3:9].[C:11](OC)(=[O:16])[C:12]([O:14][CH3:15])=[O:13].[H-].[Na+].Cl>CN(C)C=O>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8](=[O:10])[CH2:9][C:11](=[O:16])[C:12]([O:14][CH3:15])=[O:13]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 11120Dimethyl oxalateHCID 24758Sodium hydrideHCID 72864Ethanone, 1-(2-chlorophenyl)-

생성물 1

HCID 2763945Methyl 4-(2-chlorophenyl)-2,4-dioxobutanoate수율 69.1%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

반응 조건

온도
5 °C

실험 절차

In dimethylformamide (22 ml), 1-(2-chlorophenyl)ethanone (3.56 g) and dimethyl oxalate (3.26 g) were dissolved, and 60% sodium hydride suspension in oil (1.1 g) was added thereto while stirring at 5° C. The mixture was heated at a room temperature for one hour and then at 50° C. for 30 minutes. After being allowed to cool, the mixture was acidified with 2-N hydrochloric acid, and the precipitated crystal was separated by filtration, washed with water, and dried to give the title compound (3.83 g, 69%).

후처리

  1. temperatureThe mixture was heated at a room temperature for one hour
  2. temperatureto cool
  3. customthe precipitated crystal was separated by filtration
  4. washwashed with water
  5. customdried

출처 및 근거

ORD 기록
ord-fc3972b7539e4583a1e022f6a5781c0c
출처 데이터셋
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09200008B2

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