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

HRID 1647907
ノート
印刷プレビュー

反応式

HRID 1647907 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-2cb0419835394ffb85d8ca605891a9de
出典データセット
uspto-grants-1995_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05434240

反応ノート

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