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

HRID 274132노트

반응식

HRID 274132 반응식
[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]

참가 물질

4

반응물 2

HCID 729132-AminobenzonitrileHCID 118051105-Methyl-2-nitrobenzaldehyde

생성물 1

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

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-9274c858a04045b6946923ef4ef2faa2
출처 데이터셋
uspto-grants-1995_02
특허 번호
US05387684

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