Sulfuric acid magnesium salt (1:1) → 2-(4-(4-Methylpyridin-2-yl)-2-nitrobenzylidene)propionitrile

HRID 1060014노트

반응식

HRID 1060014 반응식
[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8]2[CH:15]=[CH:14][C:11]([CH:12]=O)=[C:10]([N+:16]([O-:18])=[O:17])[CH:9]=2)[CH:3]=1.C1(P(C2C=CC=CC=2)(C2C=CC=CC=2)=[C:26]([CH3:29])[C:27]#[N:28])C=CC=CC=1.S([O-])([O-])(=O)=O.[Mg+2]>C1(C)C=CC=CC=1>[CH3:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]([C:8]2[CH:15]=[CH:14][C:11]([CH:12]=[C:26]([CH3:29])[C:27]#[N:28])=[C:10]([N+:16]([O-:18])=[O:17])[CH:9]=2)[CH:3]=1

참가 물질

5

반응물 3

HCID 24083Sulfuric acid magnesium salt (1:1)HCID 136931782-(Triphenylphosphoranylidene)propanenitrileHCID 186675944-(4-Methylpyridin-2-yl)-2-nitrobenzaldehyde

생성물 1

HCID 536430862-(4-(4-Methylpyridin-2-yl)-2-nitrobenzylidene)propionitrile수율 94.4%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A suspension of 4-(4-methylpyridin-2-yl)-2-nitrobenzaldehyde (203 mg) and 2-(triphenylphosphoranylidene)propionitrile (0.45 g) in toluene (10 ml) was refluxed for 3 hours. After cooling, to the reaction mixture were added magnesium sulfate and silica gel (10 g), and the suspension was stirred for 30 minutes. The solid was removed by filtration and washed with toluene (10 ml) three times. The combined filtrate was evaporated under reduced pressure to give 2-(4-(4-methylpyridin-2-yl)-2-nitrobenzylidene)propionitrile (221 mg) as a mixture of regioisomers.

후처리

  1. temperaturewas refluxed for 3 hours
  2. temperatureAfter cooling, to the reaction mixture
  3. customThe solid was removed by filtration
  4. washwashed with toluene (10 ml) three times
  5. customThe combined filtrate was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-f5b6968ef04c480daa596c4388ac74e5
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06521643B1

반응 노트

불러오는 중…