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Potassium Carbonate → 1,2-Bis-(3,4-dicyanophenoxy)-3,5-ditertiarybutylbenzene

HRID 1647907
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HRID 1647907 반응식
[N+]([C:4]1[CH:5]=[C:6]([C:12]#[N:13])[C:7](=[CH:10][CH:11]=1)[C:8]#[N:9])([O-])=O.[C:14]([C:18]1[CH:24]=[C:23]([C:25]([CH3:28])([CH3:27])[CH3:26])[CH:22]=[C:20]([OH:21])[C:19]=1O)([CH3:17])([CH3:16])[CH3:15].[C:30](=[O:33])([O-])[O-].[K+].[K+]>CS(C)=O>[C:12]([C:6]1[CH:5]=[C:4]([CH:11]=[CH:10][C:7]=1[C:8]#[N:9])[O:21][C:20]1[CH:19]=[C:18]([C:14]([CH3:17])([CH3:16])[CH3:15])[CH:24]=[C:23]([C:25]([CH3:28])([CH3:27])[CH3:26])[C:22]=1[O:33][C:30]1[CH:11]=[CH:10][C:7]([C:8]#[N:9])=[C:6]([C:12]#[N:13])[CH:5]=1)#[N:13]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 660993,5-Di-tert-butylcatecholHCID 974431,2-Benzenedicarbonitrile, 4-nitro-

생성물 1

HCID 229064391,2-Bis-(3,4-dicyanophenoxy)-3,5-ditertiarybutylbenzene수율 86.4%

시약·촉매·용매 1

HCID 679Dimethyl Sulfoxide용매

실험 절차

3.60 g (0.02 moles plus 0.14 g excess) of 4-nitrophthalonitrile was dissolved in 50 ml anhydrous DMSO in a 100 ml three-necked flask fitted with a magnetic stirrer bar, nitrogen-gas inlet and thermometer. 2.22 g (0.01 moles) of 3,5-ditertiarybutylcatechol (supplied by Fluka) was added to the mixture followed by 5 g of anhydrous potassium carbonate. The mixture was stirred at room temperature for 24 hours and the mixture was precipitated into 400 ml water. The white solid product was washed three times with water and a further three times with methanol to yield 4.70 g (99.1% of theoretical yield) of a snow-white product which was further recrystallized from acetonitrile to yield 4.1 g of product with the formula: ##STR10## The melting point of this product was 247°-248° C. The elemental analysis for C30H26N4O2 was calc.: C, 75.94%; H, 5.48%; N, 11.81%; found: C, 76.07%; H, 5.51%; N, 1.86%.

후처리

  1. customfitted with a magnetic stirrer bar, nitrogen-gas inlet
  2. customthe mixture was precipitated into 400 ml water
  3. washThe white solid product was washed three times with water
  4. customa further three times with methanol to yield
  5. custom4.70 g (99.1% of theoretical yield) of a snow-white product which
  6. customwas further recrystallized from acetonitrile

출처 및 근거

ORD 기록
ord-2cb0419835394ffb85d8ca605891a9de
출처 데이터셋
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05434240

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