2-Chloro-4,6-diphenyl-1,3,5-triazine → 2,4-Diphenyl-1,3,5-triazine

HRID 2275955ノート

反応式

HRID 2275955 の反応式
[H-].[Na+].Cl[C:4]1[N:9]=[C:8]([C:10]2[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=2)[N:7]=[C:6]([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[N:5]=1>CN(C)C=O>[C:10]1([C:8]2[N:9]=[CH:4][N:5]=[C:6]([C:16]3[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=3)[N:7]=2)[CH:15]=[CH:14][CH:13]=[CH:12][CH:11]=1

参加物

4

反応物 2

HCID 196982-Chloro-4,6-diphenyl-1,3,5-triazineHCID 24758Sodium hydride

生成物 1

HCID 159122,4-Diphenyl-1,3,5-triazine

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

25 g (62.5 mmol) of product b) are dissolved in 200 ml of dimethylformamide under a protective-gas atmosphere, and 7.7 g of 60% NaH in mineral oil (194 mmol) are added. After 1 h at room temperature, a solution of 2-chloro-4,6-diphenyl-1,3,5-triazine (25 g, 68 mmol) in 300 ml of dimethylformamide is added dropwise. The reaction mixture is stirred at room temperature for 12 h. After this time, the reaction mixture is poured onto ice and extracted three times with dichloromethane. The combined organic phases are dried over Na2SO4 and evaporated. The residue is extracted with hot toluene, recrystallised from dichloromethane/isopropanol and finally sublimed in a high vacuum, the purity is 99.9%. The yield is 17 g (27 mmol, 44%).

後処理

  1. additionare added
  2. additionAfter this time, the reaction mixture is poured onto ice
  3. extractionextracted three times with dichloromethane
  4. dry with materialThe combined organic phases are dried over Na2SO4
  5. customevaporated
  6. extractionThe residue is extracted with hot toluene
  7. customrecrystallised from dichloromethane/isopropanol

出典と根拠

ORDレコード
ord-9fc419fa673a47d4a1cec402a14e58cd
出典データセット
uspto-grants-2015_09
特許番号
US09126970B2

反応ノート

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