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

HRID 2275955노트

반응식

HRID 2275955 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6228Dimethylformamide용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-9fc419fa673a47d4a1cec402a14e58cd
출처 데이터셋
uspto-grants-2015_09
특허 번호
US09126970B2

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