Water → 1,1-Dicyanocyclopentane

HRID 264049

反応式

HRID 264049 の反応式
[H-].[Na+].[C:3](#[N:7])[CH2:4][C:5]#[N:6].Br[CH2:9][CH2:10][CH2:11][CH2:12]Br.O>CN(C)C=O>[C:5]([C:4]1([C:3]#[N:7])[CH2:12][CH2:11][CH2:10][CH2:9]1)#[N:6]

参加物

6

反応物 4

HCID 962WaterHCID 8010MalononitrileHCID 80561,4-DibromobutaneHCID 24758Sodium hydride

生成物 1

HCID 151720351,1-Dicyanocyclopentane

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒2 回

実験手順

Sodium hydride (37.8 g; 0.94 moles) was suspended in dimethylformamide (250 mL) under an atmosphere of N2. A solution of malononitrile (30 g; 0.45 moles) and 1,4-dibromobutane 99.7 g; 0.45 moles) in dimethylformamide (150 mL) was added dropwise at such a rate so as not to exceed 30° C. The mixture was stirred for overnight, poured into H2O (500 mL), and then washed with two portions of ethyl ether. The organics were combined, washed with brine, and dried over magnesium sulfate. The drying agent was removed by filtration and the filtrate was concentrated in vacuo, leaving a bilayered liquid. The lower portion was separated (28.8 g) and identified as the desired product.

後処理

  1. customto exceed 30° C
  2. washwashed with two portions of ethyl ether
  3. washwashed with brine
  4. dry with materialdried over magnesium sulfate
  5. customThe drying agent was removed by filtration
  6. concentrationthe filtrate was concentrated in vacuo
  7. customleaving a bilayered liquid
  8. customThe lower portion was separated (28.8 g)

出典と根拠

ORDレコード
ord-3764906f1ab348f6bd1bcd3e514095c1
出典データセット
uspto-grants-1997_07
特許番号
US05646170

関連ノート

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