HCID 73605901、化合物 → 2-(4-Chlorophenyl)-1H-pyrrole-3-carbonitrile

HRID 1651684ノート

反応式

HRID 1651684 の反応式
[Cl:1][C:2]1[CH:15]=[CH:14][C:5]([C:6]([NH:10][CH2:11][CH:12]=O)=[CH:7][C:8]#[N:9])=[CH:4][CH:3]=1>FC(F)(F)C(O)=O>[Cl:1][C:2]1[CH:15]=[CH:14][C:5]([C:6]2[NH:10][CH:11]=[CH:12][C:7]=2[C:8]#[N:9])=[CH:4][CH:3]=1

参加物

3

反応物 1

HCID 73605901HCID 73605901、化合物

生成物 1

HCID 146232102-(4-Chlorophenyl)-1H-pyrrole-3-carbonitrile

試薬・触媒・溶媒 1

HCID 6422Trifluoroacetic acid溶媒

実験手順

To 108 mL of trifluoroacetic acid stirred at 23° C. is added 54.00 g (0.183 mol) of solid p-chloro-β-[(formylmethyl)amino]cinnamonitrile, diethyl acetal over a period of 45 minutes. This addition produced an exotherm to 38° C. and, 32 minutes into the addition, a solid started to precipitate. After stirring at room temperature for 30 minutes, the reaction mixture is vacuum filtered and the collected solid is washed first with trifluoroacetic acid, secondly with an ethyl acetate-hexane mixture, and finally with hexane. The yield is 16.83 g (45.4%) of an off-white solid, mp 165°-166° C. The following anal. data is from a similarly prepared sample.

後処理

  1. additionThis addition
  2. customproduced an exotherm to 38° C.
  3. addition32 minutes into the addition
  4. customto precipitate
  5. filtrationfiltered
  6. washthe collected solid is washed first with trifluoroacetic acid, secondly with an ethyl acetate-hexane mixture

出典と根拠

ORDレコード
ord-eafe58fbfa474493a67d591464a58cec
出典データセット
uspto-grants-1990_05
特許番号
US04929634

反応ノート

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