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

HRID 1033566ノート

反応式

HRID 1033566 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.

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-db0b5cf6c5a446a4bfd006f6ada49c39
出典データセット
uspto-grants-1994_05
特許番号
US05310938

反応ノート

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