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Diethyl Malonate → HCID 178516646, 화합물

HRID 1070942
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HRID 1070942 반응식
Cl.[Cl:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([Cl:9])[C:4]=1[CH2:10][C:11](=[NH:13])[NH2:12].[Na].[C:15](OCC)(=[O:22])[CH2:16][C:17](OCC)=[O:18]>C(O)C>[Cl:2][C:3]1[CH:8]=[CH:7][CH:6]=[C:5]([Cl:9])[C:4]=1[CH2:10][C:11]1[N:12]=[C:17]([OH:18])[CH:16]=[C:15]([OH:22])[N:13]=1
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참가 물질

5

반응물 3

HCID 7761Diethyl Malonate2회HCID 5360545SodiumHCID 12690064(2,6-Dichlorophenyl)ethanimidamide--hydrogen chloride (1/1)

생성물 1

HCID 178516646HCID 178516646, 화합물수율 76.4%

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

To the stirred solution of 2,6-dichlorobenzeneethanimidamide HCl (1:1), (0.0042 mol) in ethanol (20 ml), a solution of sodium (0.013 mol) in ethanol (10 ml) was added dropwise first and then propanedioic acid, diethyl ester (0.0109 mol) was added. The reaction mixture was stirred and refluxed for 4 hours and then stirred at room temperature overnight. After adding another equivalent of propanedioic acid, diethyl ester (stirring and refluxing it overnight), the solvent was evaporated and the residue was dissolved in water and acidified with 1 N HCl. The solid was filtered off, washed with water and dried, yielding 0.87 g (76.4%) of 2-[(2,6-dichloro-phenyl)methyl]-4,6-pyrimidinediol (interm. 8).

후처리

  1. temperaturerefluxed for 4 hours
  2. stirringstirred at room temperature overnight
  3. customthe solvent was evaporated
  4. dissolutionthe residue was dissolved in water
  5. filtrationThe solid was filtered off
  6. washwashed with water
  7. customdried

출처 및 근거

ORD 기록
ord-5f9d4729d7024d7eb887c95349b24019
출처 데이터셋
uspto-grants-2005_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06903213B2

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