Chloroacetonitrile → 2-Benzyl-5-cyanomethyl-2,5-diazabicyclo[2.2.1]heptane

HRID 988955

反応式

HRID 988955 の反応式
C(=O)([O-])[O-].[K+].[K+].Cl[CH2:8][C:9]#[N:10].[CH2:11]([N:18]1[CH2:23][CH:22]2[CH2:24][CH:19]1[CH2:20][NH:21]2)[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1>C1(C)C=CC=CC=1>[CH2:11]([N:18]1[CH2:23][CH:22]2[CH2:24][CH:19]1[CH2:20][N:21]2[CH2:8][C:9]#[N:10])[C:12]1[CH:13]=[CH:14][CH:15]=[CH:16][CH:17]=1

参加物

5

反応物 3

HCID 7856ChloroacetonitrileHCID 11430Potassium CarbonateHCID 5629322-Benzyl-2,5-diazabicyclo[2.2.1]heptane

生成物 1

HCID 219636452-Benzyl-5-cyanomethyl-2,5-diazabicyclo[2.2.1]heptane

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

Finely ground potassium carbonate, as well as 1.3 mL of freshly distilled chloroacetonitrile were added to a solution of 3 g of 2-benzyl-2,5-diazabicyclo[2.2.1]heptane in 40 mL of anhydrous toluene and refluxed for 10 hours with vigorous stirring. The solution was cooled, filtered and evaporated. Bulb tube distillation (boiling point: 110°-120° C. at 0.01 mbar) resulted in 3.57 g of 140 as a colorless oil (97% of the theoretical yield).

後処理

  1. temperaturerefluxed for 10 hours with vigorous stirring
  2. temperatureThe solution was cooled
  3. filtrationfiltered
  4. customevaporated
  5. distillationBulb tube distillation (boiling point: 110°-120° C. at 0.01 mbar)

出典と根拠

ORDレコード
ord-b74a3b1c9a3f4525a31d3bb55d105ccf
出典データセット
uspto-grants-2003_10
特許番号
US06638925B2

関連ノート

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