1,1-Dimethoxyethyl(dimethyl)amine → 2-(p-Fluorobenzoyl)-3-dimethylaminocrotononitrile

HRID 46554

反応式

HRID 46554 の反応式
[F:1][C:2]1[CH:12]=[CH:11][C:5]([C:6]([CH2:8][C:9]#[N:10])=[O:7])=[CH:4][CH:3]=1.CO[C:15](OC)([N:17]([CH3:19])[CH3:18])[CH3:16]>C(Cl)(Cl)Cl>[CH3:19][N:17]([CH3:18])/[C:15](/[CH3:16])=[C:8](/[C:6](=[O:7])[C:5]1[CH:11]=[CH:12][C:2]([F:1])=[CH:3][CH:4]=1)\[C:9]#[N:10]

参加物

4

反応物 2

HCID 878351,1-Dimethoxyethyl(dimethyl)amineHCID 2783172p-Fluorobenzoylacetonitrile

生成物 1

HCID 234684972-(p-Fluorobenzoyl)-3-dimethylaminocrotononitrile

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

反応条件

温度
-10 °C

実験手順

To a solution of 1.6 g. of p-fluorobenzoylacetonitrile [Pihl et al., Reakts. Sposobnost Org. Soedin. Tartu. Gos. Univ., 5 (1), 27, (1968)] in 30 ml. of chloroform, cooled to -10° C., is added 1.4 g. of N,N-dimethylacetamide dimethylacetal. The reaction mixture is stirred at -10° C. for 2 hours and the evaporated in vacuo to an oil. This oil is dissolved in 150 ml. of benzene and filtered through magnesol. The filtrate is evaporated to 50 ml. and petroleum ether is added to effect crystallization. The product is collected by filtration and then recrystallized from benzene-petroleum ether with charcoal treatment giving the desired product.

後処理

  1. additionis added 1.4 g
  2. customthe evaporated in vacuo to an oil
  3. dissolutionThis oil is dissolved in 150 ml
  4. filtrationof benzene and filtered through magnesol
  5. customThe filtrate is evaporated to 50 ml
  6. additionand petroleum ether is added to effect crystallization
  7. filtrationThe product is collected by filtration
  8. customrecrystallized from benzene-petroleum ether with charcoal treatment

出典と根拠

ORDレコード
ord-5552638b815740ab94b640be03e43efe
出典データセット
uspto-grants-1979_11
特許番号
US04173650

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