Hydrochloric Acid → HCID 57080114、化合物

HRID 973807

反応式

HRID 973807 の反応式
[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

参加物

6

反応物 4

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

生成物 1

HCID 57080114HCID 57080114、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

反応条件

温度
25 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e7d0a1bdac0446449d77f36e1bb57a4b
出典データセット
uspto-grants-1991_11
特許番号
US05064959

関連ノート

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