Aniline → 3-nitro-N-phenylpyridin-2-amine

HRID 55525ノート

反応式

HRID 55525 の反応式
Cl[C:2]1[C:7]([N+:8]([O-:10])=[O:9])=[CH:6][CH:5]=[CH:4][N:3]=1.[NH2:11][C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.C(=O)([O-])[O-].[Na+].[Na+]>C1(C)C=CC=CC=1>[N+:8]([C:7]1[C:2]([NH:11][C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[N:3][CH:4]=[CH:5][CH:6]=1)([O-:10])=[O:9]

参加物

5

反応物 3

HCID 6115AnilineHCID 10340Sodium CarbonateHCID 796132-Chloro-3-nitropyridine

生成物 1

HCID 6117993-nitro-N-phenylpyridin-2-amine収率 33.9%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

A procedure similar to that described in Preparation 66 was repeated, except that 15 g of 2-chloro-3-nitropyridine, 13.22 g of aniline and 25.07 g of sodium carbonate were reacted in 180 ml of toluene. After working up the product as described in preparation 66, the resulting crude product was purified by column chromatography through silica gel, using a 1:5 by volume mixture of ethyl acetate and hexane, to give 6.9 g of the title compound, melting at 66°-68° C.

後処理

  1. customA procedure similar to that described in Preparation 66
  2. customas described in preparation 66
  3. customthe resulting crude product was purified by column chromatography through silica gel
  4. additionby volume mixture of ethyl acetate and hexane

出典と根拠

ORDレコード
ord-ab03cc8e9cd849c6beb1ad0b306157dd
出典データセット
uspto-grants-1997_04
特許番号
US05624935

反応ノート

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