Potassium Carbonate → HCID 67032745、化合物

HRID 876625ノート

反応式

HRID 876625 の反応式
[I:1][C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][C:3]=1[OH:11].C([O-])([O-])=O.[K+].[K+].[Na+].Cl[C:20]([F:25])([F:24])C([O-])=O>CN(C=O)C.O.CCOC(C)=O>[F:24][CH:20]([F:25])[O:11][C:3]1[CH:4]=[C:5]([N+:8]([O-:10])=[O:9])[CH:6]=[CH:7][C:2]=1[I:1]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 2734985Sodium chlorodifluoroacetateHCID 186726022-Iodo-5-nitrophenol

生成物 1

HCID 67032745HCID 67032745、化合物

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 21962138N,N-Dimethylformamide--water (1/1)溶媒

反応条件

温度
110 °C

実験手順

A mixture of 2-iodo-5-nitrophenol (8.98 g), K2CO3 (18.7 g) and 2-chloro-2,2-difluoro-acetic acid sodium salt (5.17 g) in DMF-H2O (60-6 mL) was stirred at 110° C. for 3.5 h and at room temperature for 12 h. The mixture was diluted with EtOAc and washed with 1H HCl, saturated NaHCO3 aq., water and brine, and dried over anhydrous Na2SO4. The solvent was removed under reduced pressure. The resulting residue was purified by silica gel column chromatography (Hexane/EtOAc=9/1) to obtain compound aa4-1 (9.17 g) as a brown amorphous solid.

後処理

  1. washwashed with 1H HCl, saturated NaHCO3 aq., water and brine
  2. dry with materialdried over anhydrous Na2SO4
  3. customThe solvent was removed under reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography (Hexane/EtOAc=9/1)
  5. customto obtain compound aa4-1 (9.17 g) as a brown amorphous solid

出典と根拠

ORDレコード
ord-752a3b8c6cd94f12b9fe94d7a8e3c484
出典データセット
uspto-grants-2015_03
特許番号
US08987242B2

反応ノート

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