4-Fluoroaniline → HCID 12985694、化合物

HRID 2119615

反応式

HRID 2119615 の反応式
I[C:2]1[CH:3]=[N:4][N:5]([CH3:10])[C:6]=1[C:7](O)=[O:8].[F:11][C:12]1[CH:18]=[CH:17][C:15]([NH2:16])=[CH:14][CH:13]=1.C(=O)([O-])[O-].[Na+].[Na+].[OH-].[Na+]>[Cu].C(OCC)C>[F:11][C:12]1[CH:18]=[CH:17][C:15]2[NH:16][C:2]3[CH:3]=[N:4][N:5]([CH3:10])[C:6]=3[C:7](=[O:8])[C:14]=2[CH:13]=1

参加物

7

反応物 4

HCID 97314-FluoroanilineHCID 10340Sodium CarbonateHCID 14798Sodium HydroxideHCID 6736874-Iodo-1-methyl-1H-pyrazole-5-carboxylic acid

生成物 1

HCID 12985694HCID 12985694、化合物収率 61%

試薬・触媒・溶媒 2

HCID 23978Copper触媒HCID 3283Diethyl Ether溶媒

実験手順

A mixture of 4-iodo-1-methyl-1H-pyrazole-5-carboxylic acid ((Manaev, Yu. A. et al., J. Gen. Chem. USSR (Engl. Transl.), 1982, 52 (11), 2291), 500 mg, 1.98 mmol), 4-fluoroaniline (0.94 ml, 9.90 mmol), copper powder (200 mg) and 5% aqueous sodium carbonate (10 ml) was stirred for 16 h at 100° C. After cooling to room temperature, 2N aqueous sodium hydroxide (100 ml) and diethyl ether (50 ml) were added to the mixture. The mixture was filtered through a pad of Celite. The water layer was separated, washed with diethyl ether (50 ml) and acidified with concentrated hydrochloric acid. The formed precipitate was collected by filtration and dried to give 282 mg (61%) of the title compound as a white solid.

後処理

  1. filtrationThe mixture was filtered through a pad of Celite
  2. customThe water layer was separated
  3. washwashed with diethyl ether (50 ml)
  4. filtrationThe formed precipitate was collected by filtration
  5. customdried

出典と根拠

ORDレコード
ord-61298bab12dd4f30a5a7fed1e8a287bf
出典データセット
uspto-grants-2004_02
特許番号
US06686373B2

関連ノート

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