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Sodium hydride → HCID 73848368、化合物

HRID 1737210
ノート
印刷プレビュー

反応式

HRID 1737210 の反応式
[CH:1]1[C:10]2[CH2:9][CH2:8][CH2:7][CH2:6][C:5]=2[CH:4]=[CH:3][C:2]=1[C:11](=[N:13][OH:14])[CH3:12].[H-].[Na+].[Cl:17][C:18]1[N:19]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=2[CH2:31]Cl)[C:20](=[O:24])[N:21]([CH3:23])[N:22]=1>CN(C)C=O.C(OCC)(=O)C>[Cl:17][C:18]1[N:19]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=2[CH2:31][O:14][N:13]=[C:11]([C:2]2[CH:3]=[CH:4][C:5]3[CH2:6][CH2:7][CH2:8][CH2:9][C:10]=3[CH:1]=2)[CH3:12])[C:20](=[O:24])[N:21]([CH3:23])[N:22]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 24758Sodium hydrideHCID 240448HCID 240448、化合物HCID 10956231HCID 10956231、化合物

生成物 1

HCID 73848368HCID 73848368、化合物

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 8857Ethyl Acetate溶媒2 回

実験手順

To a solution of the title compound of Step C (700 mg, 3.7 mmol) in dimethylformamide (10 mL) was added sodium hydride as a 60% oil dispersion (160 mg) followed by the title compound of Step B. The mixture was stirred at room temperature for 4 h and then was diluted with ethyl acetate. The solution was washed with water and then saturated sodium chloride solution. The organic phase was dried (MgSO4) and concentrated under reduced pressure to afford an oil. Chromatography of this oil on silica gel with 20-30% ethyl acetate in hexanes afforded 1.0 g of the title compound of Step D, a compound of the invention, as an oil which solidified on standing. 1H NMR (CDCl3): δ 7.68 (m,7H), 5.2 (m,2H), 3.47 (s,3H), 2.75 (m,4H), 2.15 (s,3H), 1.78 (m,4H). This material was used in the preparation of Example 4 without further characterization.

後処理

  1. washThe solution was washed with water
  2. dry with materialThe organic phase was dried (MgSO4)
  3. concentrationconcentrated under reduced pressure
  4. customto afford an oil

出典と根拠

ORDレコード
ord-1db286a674804a7498f6b482b84c4373
出典データセット
uspto-grants-1999_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05962436

反応ノート

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