2-Aminobenzonitrile → 2-[N-(5-methyl-2-nitrobenzylidene)amino]benzonitrile

HRID 274132ノート

反応式

HRID 274132 の反応式
[NH2:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]#[N:5].[CH3:10][C:11]1[CH:12]=[CH:13][C:14]([N+:19]([O-:21])=[O:20])=[C:15]([CH:18]=1)[CH:16]=O>C1(C)C=CC=CC=1>[CH3:10][C:11]1[CH:12]=[CH:13][C:14]([N+:19]([O-:21])=[O:20])=[C:15]([CH:18]=1)[CH:16]=[N:1][C:2]1[CH:9]=[CH:8][CH:7]=[CH:6][C:3]=1[C:4]#[N:5]

参加物

4

反応物 2

HCID 729132-AminobenzonitrileHCID 118051105-Methyl-2-nitrobenzaldehyde

生成物 1

HCID 200945252-[N-(5-methyl-2-nitrobenzylidene)amino]benzonitrile収率 62.1%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Toluene (167 ml) and 2-aminobenzonitrile (19.7 g, 167 mmol) were added to 5-methyl-2-nitrobenzaldehyde (27.5 g, 167 mmol) as obtained in Reference Example 1, and the mixture was stirred and refluxed for 14 hours, followed by cooling. The resultant crystals were filtered off, washed with a mixed solvent of hexane/toluene (2:1, 150 ml) and hexane (150 ml) twice to give 27.5 g of 2-[N-(5-methyl-2-nitrobenzylidene)amino]benzonitrile. In addition, the solid precipitated from the filtrate was filtered off and washed with hexane (100 ml and 50 ml) to give 10.0 g of the compound.

後処理

  1. customas obtained in Reference Example 1
  2. temperaturerefluxed for 14 hours
  3. temperatureby cooling
  4. filtrationThe resultant crystals were filtered off
  5. washwashed with a mixed solvent of hexane/toluene (2:1, 150 ml) and hexane (150 ml) twice

出典と根拠

ORDレコード
ord-9274c858a04045b6946923ef4ef2faa2
出典データセット
uspto-grants-1995_02
特許番号
US05387684

反応ノート

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