Dimethylformamide → 5-[(4-Chlorophenyl)methoxy]-2-nitropyridine

HRID 1995820ノート

反応式

HRID 1995820 の反応式
[OH:1][C:2]1[CH:3]=[CH:4][C:5]([N+:8]([O-:10])=[O:9])=[N:6][CH:7]=1.C([O-])([O-])=O.[K+].[K+].CN(C=O)C.[Cl:22][C:23]1[CH:30]=[CH:29][C:26]([CH2:27]Cl)=[CH:25][CH:24]=1>C(Cl)(Cl)Cl>[Cl:22][C:23]1[CH:30]=[CH:29][C:26]([CH2:27][O:1][C:2]2[CH:3]=[CH:4][C:5]([N+:8]([O-:10])=[O:9])=[N:6][CH:7]=2)=[CH:25][CH:24]=1

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 77231-Chloro-4-(chloromethyl)benzeneHCID 11430Potassium CarbonateHCID 27628576-Nitropyridin-3-ol

生成物 1

HCID 204861295-[(4-Chlorophenyl)methoxy]-2-nitropyridine

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

A mixture of 5-hydroxy-2-nitropyridine (7 g), K2CO3 (6.9 g) of DMF (100 ml) is stirred for about 10 minutes. To the mixture is added 4-chlorobenzyl chloride (8.1 g) in portions over about 15 minutes. The reaction mixture is stirred about 16 hours and then heated to 45° for about 30 minutes. After cooling, the reaction is diluted with CHCl3, washed with water and saturated NaCl, dried (Na2SO4) and stripped. The crystalline solid is washed with 20% ethyl acetate/hexane, giving 5-(4-chlorobenzyloxy)-2-nitropyridine.

後処理

  1. stirringThe reaction mixture is stirred about 16 hours
  2. temperatureheated to 45° for about 30 minutes
  3. temperatureAfter cooling
  4. washwashed with water and saturated NaCl
  5. dry with materialdried (Na2SO4)
  6. washThe crystalline solid is washed with 20% ethyl acetate/hexane

出典と根拠

ORDレコード
ord-d7b70505cb554565b000a38fca5fc509
出典データセット
uspto-grants-1983_09
特許番号
US04406690

反応ノート

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