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Hydrochloric Acid → HCID 17816478、化合物

HRID 2249697
ノート
印刷プレビュー

反応式

HRID 2249697 の反応式
[Br:1][C:2]1[C:10]2[NH:9][C:8](=[O:11])[NH:7][C:6]=2[CH:5]=[C:4]([Br:12])[C:3]=1[C:13]([O:15][CH3:16])=[O:14].[H-].[Na+].[CH2:19](Br)[CH2:20][CH:21]([CH3:23])[CH3:22].Cl>CN(C)C=O.O.C(OCC)(=O)C>[Br:1][C:2]1[C:10]2[N:9]([CH2:19][CH2:20][CH:21]([CH3:23])[CH3:22])[C:8](=[O:11])[N:7]([CH2:10][CH2:2][CH:3]([CH3:13])[CH3:4])[C:6]=2[CH:5]=[C:4]([Br:12])[C:3]=1[C:13]([O:15][CH3:16])=[O:14]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 78911-Bromo-3-methylbutaneHCID 24758Sodium hydrideHCID 17816488HCID 17816488、化合物

生成物 1

HCID 17816478HCID 17816478、化合物

試薬・触媒・溶媒 3

HCID 962Water溶媒
HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

反応条件

温度
55 °C

実験手順

In 10 ml of N,N-dimethylformamide are suspended 0.95 g of methyl 4,6-dibromo-2-oxo-2,3-dihydro-1H-benzimidazole-5-carboxylate, 0.24 g of 60% sodium hydride and 0.7 ml of isopentyl bromide. The suspension is stirred at 50-60° C. for 3 hours. The reaction mixture is added to a mixture of ethyl acetate and water, pH is adjusted to 2 with 2 mol/L hydrochloric acid, and the organic layer is separated. The organic layer thus obtained is washed with water and saturated aqueous solution of sodium chloride successively and dried over anhydrous magnesium sulfate, and then the solvent is distilled off under reduced pressure. Thus, 0.71 g of methyl 4,6-dibromo-1,3-diisopentyl-2-oxo-2,3-dihydro-1H-benzimidazole-5-carboxylate is obtained as a light brown-colored solid product.

後処理

  1. customthe organic layer is separated
  2. customThe organic layer thus obtained
  3. washis washed with water and saturated aqueous solution of sodium chloride successively
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationthe solvent is distilled off under reduced pressure

出典と根拠

ORDレコード
ord-8be4fc6a151945349a1ce116a9ce0165
出典データセット
uspto-grants-2008_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07314888B1

反応ノート

読み込み中…

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