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N,N-Dimethyl-beta-alaninamide → 3-{3-[5-(2,6-Dimethyl-pyridin-4-yl)-4-methyl-thiazol-2-yl]-ureido}-N,N-dimethyl-propionamide

HRID 1951226
ノート
印刷プレビュー

反応式

HRID 1951226 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([C:8]2[S:12][C:11]([NH:13][C:14]([N:16]3[CH:20]=[CH:19]N=C3)=[O:15])=[N:10][C:9]=2[CH3:21])[CH:5]=[C:4]([CH3:22])[N:3]=1.NCC[C:26]([N:28]([CH3:30])[CH3:29])=[O:27]>CN(C=O)C>[CH3:22][C:4]1[CH:5]=[C:6]([C:8]2[S:12][C:11]([NH:13][C:14](=[O:15])[NH:16][CH2:20][CH2:19][C:26]([N:28]([CH3:30])[CH3:29])=[O:27])=[N:10][C:9]=2[CH3:21])[CH:7]=[C:2]([CH3:1])[N:3]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 12742480N,N-Dimethyl-beta-alaninamideHCID 86610333Imidazole-1-carboxylic acid [5-(2,6-dimethyl-pyridin-4-yl)-4-methyl-thiazol-2-yl]-amide

生成物 1

HCID 112913913-{3-[5-(2,6-Dimethyl-pyridin-4-yl)-4-methyl-thiazol-2-yl]-ureido}-N,N-dimethyl-propionamide

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

To a stirred solution of imidazole-1-carboxylic acid [5-(2,6-dimethyl-pyridin-4-yl)-4-methyl-thiazol-2-yl]-amide (Intermediate BA) (0.05 g, 0.16 mmol) in DMF (1.5 ml) under an inert atmosphere is added 3-amino-N,N-dimethyl-propionamide (Amine) (0.018 g, 0.16 mmol). The reaction mixture is stirred at room temperature for 18 hours. The solvent is removed in vacuo and the resulting crude residue is dissolved in THF and passed through a plug of polymer supported isocyanate resin (0.5 g, pre-washed with THF). The solution is concentrated in vacuo and the crude residue is trituated with ether-ethyl acetate to afford the titled compound as a yellow solid.

後処理

  1. customThe solvent is removed in vacuo
  2. dissolutionthe resulting crude residue is dissolved in THF
  3. concentrationThe solution is concentrated in vacuo

出典と根拠

ORDレコード
ord-dc7d044396cb4061bbc5120b444a773b
出典データセット
uspto-grants-2013_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08404684B2

反応ノート

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