HCID 73605901, 화합물 → 2-(4-Chlorophenyl)-1H-pyrrole-3-carbonitrile

HRID 1033566노트

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HRID 1033566 반응식
[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

참가 물질

3

반응물 1

HCID 73605901HCID 73605901, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-db0b5cf6c5a446a4bfd006f6ada49c39
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05310938

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