1-Naphthaleneacetonitrile → 1-Naphthylmalononitrile

HRID 1594994ノート

反応式

HRID 1594994 の反応式
[C:1]1([CH2:11][C:12]#[N:13])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1.ClC1C=CC=CC=1CS[C:19]#[N:20].C([N-]C(C)C)(C)C.[Li+].[OH-].[Na+]>C1C=CC=CC=1>[C:1]1([CH:11]([C:19]#[N:20])[C:12]#[N:13])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[CH:4]=[CH:3][CH:2]=1

参加物

6

反応物 4

HCID 85961-NaphthaleneacetonitrileHCID 14798Sodium HydroxideHCID 2867232-Chlorobenzyl ThiocyanateHCID 2724682Lithium diisopropylamide

生成物 1

HCID 109103631-Naphthylmalononitrile

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

With stirring and cooling, 0.3 mol of 1-naphthylaceto-nitrile and then, dropwise, 0.6 mol of 2-chlorobenzyl thiocyanate are added to a solution of 0.65 mol of lithium diisopropylamide in benzene. After one hour, the reaction mixture is introduced into 1 l of 0.3 molar NaOH, and the mixture is allowed to stand for a while and then the two phases which are formed are separated. The aqueous solution is neutralized by adding hydrochloric acid and allowed to stand overnight. The precipitated product is filtered off with suction, dried and purified by recrystallization from ethanol.

後処理

  1. temperaturecooling
  2. customthe two phases which are formed
  3. customare separated
  4. additionby adding hydrochloric acid
  5. waitto stand overnight
  6. filtrationThe precipitated product is filtered off with suction
  7. customdried
  8. custompurified by recrystallization from ethanol

出典と根拠

ORDレコード
ord-2077ac4c27f64b2e8445d3db60f6cb2d
出典データセット
uspto-grants-2001_09
特許番号
US06284889B1

反応ノート

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