Sodium hydride → 3-(4-Tert-butylphenyl)-1-[(2-chloropyridin-4-yl)methyl]-5,5-dimethylimidazolidine-2,4-dione

HRID 546583

反応式

HRID 546583 の反応式
[H-].[Na+].[C:3]([C:7]1[CH:12]=[CH:11][C:10]([N:13]2[C:17](=[O:18])[C:16]([CH3:20])([CH3:19])[NH:15][C:14]2=[O:21])=[CH:9][CH:8]=1)([CH3:6])([CH3:5])[CH3:4].[Cl:22][C:23]1[CH:28]=[C:27]([CH2:29]Cl)[CH:26]=[CH:25][N:24]=1>CN(C)C=O.O>[C:3]([C:7]1[CH:8]=[CH:9][C:10]([N:13]2[C:17](=[O:18])[C:16]([CH3:20])([CH3:19])[N:15]([CH2:29][C:27]3[CH:26]=[CH:25][N:24]=[C:23]([Cl:22])[CH:28]=3)[C:14]2=[O:21])=[CH:11][CH:12]=1)([CH3:6])([CH3:4])[CH3:5]

参加物

6

反応物 3

HCID 24758Sodium hydrideHCID 111265732-Chloro-4-(chloromethyl)pyridineHCID 576259723-(4-Tert-butylphenyl)-5,5-dimethyl-imidazolidine-2,4-dione

生成物 1

HCID 576259713-(4-Tert-butylphenyl)-1-[(2-chloropyridin-4-yl)methyl]-5,5-dimethylimidazolidine-2,4-dione収率 63.5%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

To a suspension of 1.1 g of sodium hydride in 40 mL of dimethylformamide under argon are successively added 4.9 g of 3-(4-tert-butylphenyl)-5,5-dimethylimidazolidine-2,4-dione obtained in stage c) of Example 1 and 4.55 g of 2-chloro-4-(chloromethyl)pyridine. The reaction mixture is stirred for 48 hours at room temperature and then diluted with 260 mL of water. The solid formed is filtered off, rinsed with diisopropyl ether and dried to give 4.61 g of 3-(4-tert-butylphenyl)-1-[(2-chloropyridin-4-yl)methyl]-5,5-dimethylimidazolidine-2,4-dione in the form of a beige-coloured powder, the characteristics of which are as follows:

後処理

  1. customThe solid formed
  2. filtrationis filtered off
  3. washrinsed with diisopropyl ether
  4. customdried

出典と根拠

ORDレコード
ord-7c53bd76a9bd4d68940eca962bf2a48f
出典データセット
uspto-grants-2011_05
特許番号
US07935819B2

関連ノート

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