(4-Chloro-2-fluoro-5-propan-2-yloxyphenyl)hydrazine → 3,3,3-Trifluoro-2-oxopropanal 1-(4-chloro-2-fluoro-5-isopropoxyphenylhydrazone)

HRID 1274513ノート

反応式

HRID 1274513 の反応式
C([O-])(=O)C.[Na+].Cl[CH:7](Cl)[C:8]([C:10]([F:13])([F:12])[F:11])=[O:9].[F:15][C:16]1[CH:21]=[C:20]([Cl:22])[C:19]([O:23][CH:24]([CH3:26])[CH3:25])=[CH:18][C:17]=1[NH:27][NH2:28]>O.C(OCC)C>[Cl:22][C:20]1[C:19]([O:23][CH:24]([CH3:25])[CH3:26])=[CH:18][C:17]([NH:27][N:28]=[CH:7][C:8](=[O:9])[C:10]([F:13])([F:12])[F:11])=[C:16]([F:15])[CH:21]=1

参加物

6

反応物 3

HCID 185080(4-Chloro-2-fluoro-5-propan-2-yloxyphenyl)hydrazineHCID 517045Sodium AcetateHCID 27790203,3-Dichloro-1,1,1-trifluoroacetone

生成物 1

HCID 691414303,3,3-Trifluoro-2-oxopropanal 1-(4-chloro-2-fluoro-5-isopropoxyphenylhydrazone)収率 81.8%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

To a solution of 5.3 g of sodium acetate dissolved in 100 ml of water was added 4.4 g of 1,1-dichloro-3,3,3-trifluoroacetone under ice cooling, and the reaction was allowed to proceed at 90° C. for 30 minutes. The reaction solution was left cooling to room temperature, to which a solution of 5.8 g of 2-fluoro-4-chloro-5-isopropoxyphenylhydrazine dissolved in 20 ml of diethyl ether was added, and the mixture was stirred at room temperature for 1 hour. The organic layer was separated, washed once with 10 ml of saturated aqueous sodium chloride solution, dried with anhydrous magnesium sulfate, and evaporated to remove the diethyl ether to give 6.5 g of 3,3,3-trifluoro-2-oxopropanal 1-(4-chloro-2-fluoro-5-isopropoxyphenylhydrazone), compound 3-3.

後処理

  1. waitThe reaction solution was left
  2. additionwas added
  3. customThe organic layer was separated
  4. washwashed once with 10 ml of saturated aqueous sodium chloride solution
  5. dry with materialdried with anhydrous magnesium sulfate
  6. customevaporated
  7. customto remove the diethyl ether

出典と根拠

ORDレコード
ord-d3871d39c0784dab8942e284a89243c4
出典データセット
uspto-grants-2000_12
特許番号
US06156891

反応ノート

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