Acetic Acid → 1-(2,6-Dichlorophenyl)-1H-pyrrole

HRID 2427082노트

반응식

HRID 2427082 반응식
[Cl:1][C:2]1[CH:8]=[CH:7][CH:6]=[C:5]([Cl:9])[C:3]=1[NH2:4].CO[CH:12]1[CH2:16][CH2:15][CH:14](OC)O1.C(O)(=O)C>O>[Cl:1][C:2]1[CH:8]=[CH:7][CH:6]=[C:5]([Cl:9])[C:3]=1[N:4]1[CH:12]=[CH:16][CH:15]=[CH:14]1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 118462,6-DichloroanilineHCID 790982,5-Dimethoxytetrahydrofuran

생성물 1

HCID 207882021-(2,6-Dichlorophenyl)-1H-pyrrole수율 83.3%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 5 g of 2,6-dichloroaniline, 4.5 g of 2,5-dimethoxytetrahydrofuran and 30 ml of acetic acid was heated to reflux for 10 hours. The reaction mixture was allowed to cool, poured into water, and extracted with ethyl acetate two times. The organic layers were combined, washed successively with water and an aqueous saturated sodium chloride solution, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The resulting residue was subjected to silica gel chromatography to obtain 5.45 g of 1-(2,6-dichlorophenyl)-1H-pyrrole of the formula:

후처리

  1. temperaturewas heated
  2. temperatureto reflux for 10 hours
  3. temperatureto cool
  4. extractionextracted with ethyl acetate two times
  5. washwashed successively with water
  6. dry with materialan aqueous saturated sodium chloride solution, dried over anhydrous sodium sulfate
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-a6b6043e2d0f491995891e3a03b3c4b9
출처 데이터셋
uspto-grants-2011_06
특허 번호
US07968573B2

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