Water → HCID 12833268、化合物

HRID 1074851ノート

反応式

HRID 1074851 の反応式
[H-].[Na+].[N+:3]([C:6]1[CH:7]=[C:8]([NH:14][C:15](=[O:19])[CH2:16][CH2:17]Cl)[C:9]([CH3:13])=[CH:10][C:11]=1[CH3:12])([O-:5])=[O:4].O>CS(C)=O.O1CCCC1>[N+:3]([C:6]1[CH:7]=[C:8]([N:14]2[CH2:17][CH2:16][C:15]2=[O:19])[C:9]([CH3:13])=[CH:10][C:11]=1[CH3:12])([O-:5])=[O:4]

参加物

6

反応物 3

HCID 962WaterHCID 24758Sodium hydrideHCID 12833267HCID 12833267、化合物

生成物 1

HCID 12833268HCID 12833268、化合物

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

5 g of sodium hydride (in the form of a 55% strength dispersion in oil) are stirred in 100 ml of dimethylsulphoxide until no further evolution of gas can be detected. 21.5 g (0.084 mol) of N-(3-nitro-4,6-dimethylphenyl)-β-chloropropionamide, suspended in 500 ml of tetrahydrofurane, are then added in the course of 5-10 minutes. The reaction temperature is kept at 15° for 1/2 an hour and water is then added dropwise in order to destroy excess sodium hydride. The reaction solution is taken up in methylene chloride and washed with water and saturated NaCl solution, dried (MgSO4) and evaporated. The crude product is subjected to fractional filtration on silica gel in chloroform. This gives 14.5 g (78%) of product; melting point 102°.

後処理

  1. additionare then added in the course of 5-10 minutes
  2. additionis then added dropwise in order
  3. customto destroy excess sodium hydride
  4. washwashed with water and saturated NaCl solution
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. filtrationThe crude product is subjected to fractional filtration on silica gel in chloroform

出典と根拠

ORDレコード
ord-63b944924af14706af92eac2cf0fcfbd
出典データセット
uspto-grants-1983_07
特許番号
US04394156

反応ノート

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