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Diethyl Malonate → HCID 178516646、化合物

HRID 2305415
ノート
印刷プレビュー

反応式

HRID 2305415 の反応式
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
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7761Diethyl Malonate2 回HCID 5360545SodiumHCID 12690064(2,6-Dichlorophenyl)ethanimidamide--hydrogen chloride (1/1)

生成物 1

HCID 178516646HCID 178516646、化合物収率 76.4%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-f1eedc03c03d40618ba5492f7564353c
出典データセット
uspto-grants-2002_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06440986B2

反応ノート

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