Hydrochloric Acid → HCID 57080114, 화합물

HRID 973807

반응식

HRID 973807 반응식
[C:1]([C:3]1[CH:4]=[C:5]([CH:12]=[CH:13][CH:14]=1)[CH:6]=[CH:7][C:8]([O:10][CH3:11])=[O:9])#[N:2].[Cl:15][C:16]([Cl:20])([Cl:19])[C:17]#[N:18].[Br-].[Al+3].[Br-].[Br-].[ClH:25]>ClCCl>[Cl:15][C:16]([Cl:20])([Cl:19])[C:17]1[N:18]=[C:17]([C:16]([Cl:19])([Cl:15])[Cl:25])[N:18]=[C:1]([C:3]2[CH:4]=[C:5]([CH:12]=[CH:13][CH:14]=2)[CH:6]=[CH:7][C:8]([O:10][CH3:11])=[O:9])[N:2]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 11011TrichloroacetonitrileHCID 166749BromhydrolHCID 53396017Methyl 3-(3-cyanophenyl)prop-2-enoate

생성물 1

HCID 57080114HCID 57080114, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
25 °C

실험 절차

Methyl 3-cyanocinnamate (42 pw) is added to a mixture of trichloroacetonitrile (194.4 pw) and aluminum bromide (7.2 pw) in the absence of moisture and at about 25° C. Hydrogen chloride is then introduced over a period of 3 hours with stirring, while keeping the temperature constant. Stirring is discontinued, and the mixture is allowed to react further overnight. In this step, too, a constant temperature of 25° C. is maintained. The solidified mixture is dissolved in 800 pw of dichloromethane, washed with water, and the organic phase is dried over sodium sulfate. Evaporation of the solvent gives a white residue, which is recrystallized from methanol or benzene.

후처리

  1. stirringStirring
  2. customto react further overnight
  3. washwashed with water
  4. dry with materialthe organic phase is dried over sodium sulfate
  5. customEvaporation of the solvent
  6. customgives a white residue, which
  7. customis recrystallized from methanol or benzene

출처 및 근거

ORD 기록
ord-e7d0a1bdac0446449d77f36e1bb57a4b
출처 데이터셋
uspto-grants-1991_11
특허 번호
US05064959

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