Malononitrile → Dihydro-2H-pyran-4,4(3H)-dicarbonitrile

HRID 651736

反応式

HRID 651736 の反応式
Cl[CH:2](Cl)[CH2:3][O:4][CH2:5][CH:6](Cl)Cl.[C:10](#[N:14])[CH2:11][C:12]#[N:13].C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[O:4]1[CH2:5][CH2:6][C:11]([C:10]#[N:14])([C:12]#[N:13])[CH2:2][CH2:3]1

参加物

5

反応物 3

HCID 8010MalononitrileHCID 11430Potassium CarbonateHCID 623831,1'-Oxybis(2,2-dichloroethane)

生成物 1

HCID 14537194Dihydro-2H-pyran-4,4(3H)-dicarbonitrile収率 51.7%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

A mixture of 28.6 g of dichloroethyl ether, 13.2 g of malononitrile, 55.28 g of potassium carbonate and 800 ml of acetonitrile was refluxed on a steam bath for 24 hours, then filtered while hot. The filtrate was evaporated and the residue crystallized with charcoal treatment from 100 ml of ethanol, giving 9.5 g of tetrahydro-4H-pyran-4,4-dicarbonitrile as colorless plates, mp 110-112° C.

後処理

  1. temperaturewas refluxed on a steam bath for 24 hours
  2. filtrationfiltered while hot
  3. customThe filtrate was evaporated
  4. customthe residue crystallized with charcoal treatment from 100 ml of ethanol

出典と根拠

ORDレコード
ord-2e4a3b4ca2244565a6f7509696dea21d
出典データセット
uspto-grants-2001_08
特許番号
US06281365B1

関連ノート

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