Pyrazole → 1-(3-nitrophenyl)-1H-pyrazole

HRID 581946노트

반응식

HRID 581946 반응식
I[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([N+:8]([O-:10])=[O:9])[CH:3]=1.[NH:11]1[CH:15]=[CH:14][CH:13]=[N:12]1.C(=O)([O-])[O-].[K+].[K+]>CN1CCCC1=O>[N+:8]([C:4]1[CH:3]=[C:2]([N:11]2[CH:15]=[CH:14][CH:13]=[N:12]2)[CH:7]=[CH:6][CH:5]=1)([O-:10])=[O:9]

참가 물질

5

반응물 3

HCID 1048PyrazoleHCID 11430Potassium CarbonateHCID 125741-Iodo-3-nitrobenzene

생성물 1

HCID 121007811-(3-nitrophenyl)-1H-pyrazole수율 96%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

반응 조건

온도
180 °C

실험 절차

A mixture of 1-iodo-3-nitrobenzene (18.7 g, 75 mmol), pyrazol (7.66 g, 113 mmol), potassium carbonate (11.2 g, 81 mmol) and catalytic amounts of cuprous iodide and copper-bronze in dry N-methyl-2-pyrrolidone (50 ml) is heated to 180° C. for 4.5 hours. After cooling the mixture is filtered through celite. The filtrate is poured into ice water (700 ml) and the product is filtered off, washed with water and dried to yield 13.57 g. Yield: 96%. Mp 85-87° C.

후처리

  1. temperatureAfter cooling the mixture
  2. filtrationis filtered through celite
  3. additionThe filtrate is poured into ice water (700 ml)
  4. filtrationthe product is filtered off
  5. washwashed with water
  6. customdried
  7. customto yield 13.57 g

출처 및 근거

ORD 기록
ord-54e41fdecb8e4021b5ecfe8c075c7e9d
출처 데이터셋
uspto-grants-1999_07
특허 번호
US05922724

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