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Diethyl Malonate → 3-[1-(4-Nitrobenzyl)benzimidazol-2-yl]-2-(carboethoxy)propanoic acid, ethyl ester

HRID 1638560
ノート
印刷プレビュー

反応式

HRID 1638560 の反応式
[Na].C(C(CC)(C([O-])=O)C([O-])=O)C.[H-].[Na+].[C:15]([O:23][CH2:24][CH3:25])(=[O:22])[CH2:16][C:17]([O:19][CH2:20][CH3:21])=[O:18].[N+:26]([C:29]1[CH:46]=[CH:45][C:32]([CH2:33][N:34]2[C:38]3[CH:39]=[CH:40][CH:41]=[CH:42][C:37]=3[N:36]=[C:35]2[CH2:43]Cl)=[CH:31][CH:30]=1)([O-:28])=[O:27]>CN(C=O)C.C(OCC)(=O)C>[N+:26]([C:29]1[CH:46]=[CH:45][C:32]([CH2:33][N:34]2[C:38]3[CH:39]=[CH:40][CH:41]=[CH:42][C:37]=3[N:36]=[C:35]2[CH2:43][CH:16]([C:17]([O:19][CH2:20][CH3:21])=[O:18])[C:15]([O:23][CH2:24][CH3:25])=[O:22])=[CH:31][CH:30]=1)([O-:28])=[O:27]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 7761Diethyl MalonateHCID 24758Sodium hydrideHCID 5360545SodiumHCID 69515632,2-DiethylpropanedioateHCID 14722476HCID 14722476、化合物

生成物 1

HCID 147224773-[1-(4-Nitrobenzyl)benzimidazol-2-yl]-2-(carboethoxy)propanoic acid, ethyl ester

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒

実験手順

The sodium salt of diethylmalonate was generated from 0.35 g of NaH (50% oil dispersion) and 1.1 mL of diethyl malonate in 15 mL of dried DMF with ice cooling. To the above mixture was added 2 g of 1-(4-nitrobenzyl)-2-chloromethylbenzimidazole and the mixture was stirred at room temperature for 18 hours. The reaction mixture was diluted with ethyl acetate, washed with water, dried and concentrated in vacuo. The crude produce was purified by flash column chromatography (hexane/ethyl acetate, 1:1) to give a yellowish thick oil which was crystallized from absolute ethanol to give a white solid; m.p. 135°.

後処理

  1. washwashed with water
  2. customdried
  3. concentrationconcentrated in vacuo
  4. customThe crude produce
  5. customwas purified by flash column chromatography (hexane/ethyl acetate, 1:1)
  6. customto give a yellowish thick oil which
  7. customwas crystallized from absolute ethanol
  8. customto give a white solid

出典と根拠

ORDレコード
ord-6fbc542354b249f29e5a898a781a51d8
出典データセット
uspto-grants-1989_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04880804

反応ノート

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