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

HRID 46554

반응식

HRID 46554 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6212Chloroform용매

반응 조건

온도
-10 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-5552638b815740ab94b640be03e43efe
출처 데이터셋
uspto-grants-1979_11
특허 번호
US04173650

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