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Water → 2-(4-Chlorophenylmethylamino)-3-nitro-5-chloropyridine

HRID 1493319
ノート
印刷プレビュー

反応式

HRID 1493319 の反応式
[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][NH2:7])=[CH:4][CH:3]=1.Cl[C:11]1[C:16]([N+:17]([O-:19])=[O:18])=[CH:15][C:14]([Cl:20])=[CH:13][N:12]=1.O>C1(C)C(C)=CC=CC=1.CC1C=CC(CC)=CN=1>[Cl:1][C:2]1[CH:9]=[CH:8][C:5]([CH2:6][NH:7][C:11]2[C:16]([N+:17]([O-:19])=[O:18])=[CH:15][C:14]([Cl:20])=[CH:13][N:12]=2)=[CH:4][CH: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

6

反応物 3

HCID 962WaterHCID 660364-ChlorobenzylamineHCID 80633312,5-Dichloro-3-nitropyridine

生成物 1

HCID 110664382-(4-Chlorophenylmethylamino)-3-nitro-5-chloropyridine収率 87%

試薬・触媒・溶媒 2

HCID 7237O-Xylene溶媒HCID 77285-Ethyl-2-methylpyridine
溶媒

実験手順

A solution of 20.9 g of 4-chlorobenzylamine and 15.7 g of 2,5-dichloro-3-nitropyridine in 250 ml of xylene and 20 ml of 2-methyl-5-ethylpyridine is refluxed for 30 hours. After cooling, water is added to the reaction mixture, the resulting mixture is then extracted with ethyl acetate and the organic phase is washed with a dilute solution of hydrochloric acid and dried over magnesium sulfate. The solvent is evaporated off under vacuum and the residue obtained crystallizes from isopropyl ether to give 21.1 g of 2-(4-chlorophenylmethylamino)-3-nitro-5-chloropyridine in the form of crystals melting at 120° C.

後処理

  1. temperatureAfter cooling
  2. extractionthe resulting mixture is then extracted with ethyl acetate
  3. washthe organic phase is washed with a dilute solution of hydrochloric acid
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent is evaporated off under vacuum
  6. customthe residue obtained
  7. customcrystallizes from isopropyl ether

出典と根拠

ORDレコード
ord-099b8fed300d4b5fbc6c4c4fd4c1d31f
出典データセット
uspto-grants-1991_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05021443

反応ノート

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