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

HRID 581946ノート

反応式

HRID 581946 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 121007811-(3-nitrophenyl)-1H-pyrazole収率 96%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
180 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-54e41fdecb8e4021b5ecfe8c075c7e9d
出典データセット
uspto-grants-1999_07
特許番号
US05922724

反応ノート

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