Sulfuryl chloride → HCID 15010168, 화합물

HRID 1033574노트

반응식

HRID 1033574 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([C:8]2[NH:9][CH:10]=[CH:11][C:12]=2[C:13]#[N:14])=[CH:4][CH:3]=1.S(Cl)([Cl:18])(=O)=O>C(O)(=O)C>[Cl:18][C:10]1[NH:9][C:8]([C:5]2[CH:4]=[CH:3][C:2]([Cl:1])=[CH:7][CH:6]=2)=[C:12]([C:13]#[N:14])[CH:11]=1

참가 물질

4

반응물 2

HCID 24648Sulfuryl chlorideHCID 146232102-(4-Chlorophenyl)-1H-pyrrole-3-carbonitrile

생성물 1

HCID 15010168HCID 15010168, 화합물수율 58%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

To a 35° C. magnetically stirred solution of 2.40 g (11.8 mmol., 1.00 equivalent) of 2-(p-chlorophenyl)pyrrole-3-carbonitrile, and 65 mL of glacial acetic acid is added dropwise by syringe 0.75 mL (1.26 g, 9.34 mmol., 0.79 equivalent) of sulfuryl chloride over a period of 5 minutes. Approximately 5 minutes after the completion of the addition, a solid precipitated out of the reaction solution. After stirring at room temperature for 45 minutes, the reaction mixture is filtered and the collected solid is washed well with cold acetic acid to give 2.08 g (74% crude yield) of an off-white solid. This solid is recrystallized from 75 mL of hot acetic acid to give 1.63 g (58% yield) of 97 wt % pure. Product mp 258.5°-261° C.

후처리

  1. additionApproximately 5 minutes after the completion of the addition
  2. customa solid precipitated out of the reaction solution
  3. filtrationthe reaction mixture is filtered
  4. washthe collected solid is washed well with cold acetic acid
  5. customto give 2.08 g (74% crude yield) of an off-white solid
  6. customThis solid is recrystallized from 75 mL of hot acetic acid
  7. customto give 1.63 g (58% yield) of 97 wt % pure

출처 및 근거

ORD 기록
ord-650da2ec3094428286dc1cfa73b75719
출처 데이터셋
uspto-grants-1994_05
특허 번호
US05310938

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