Tin tetrachloride → HCID 44139769、化合物

HRID 1896984ノート

反応式

HRID 1896984 の反応式
[O:1]([C:8]1[C:13]([CH3:14])=[CH:12][C:11]([N+:15]([O-])=O)=[C:10]([CH3:18])[CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[Sn](Cl)(Cl)(Cl)Cl.C([O-])(O)=O.[Na+]>O1CCOCC1.Cl>[O:1]([C:8]1[CH:9]=[C:10]([CH3:18])[C:11](=[CH:12][C:13]=1[CH3:14])[NH2:15])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 3

HCID 24287Tin tetrachlorideHCID 516892Sodium BicarbonateHCID 685941194-Phenoxy-2,5-dimethylnitrobenzene

生成物 1

HCID 44139769HCID 44139769、化合物収率 73.2%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 312751,4-Dioxane溶媒

実験手順

A solution of 12.3 g (50 mmol) of 4-phenoxy-2,5-dimethylnitrobenzene in 150 ml of dioxane and 150 ml of hydrochloric acid was admixed at room temperature with 34.1 g (151 mmol) of tin chloride. After 10 h of stirring at room temperature, the mixture was neutralized with aqueous NaHCO3 solution and extracted repeatedly with dichloromethane. Drying of the combined organic phases over Na2SO4 and evaporation of the solvent gave 7.9 g (99.5% purity, 73.2% yield) of the product; log P(HCOOH)=1.92.

後処理

  1. extractionextracted repeatedly with dichloromethane
  2. dry with materialDrying of the combined organic phases over Na2SO4 and evaporation of the solvent
  3. customgave 7.9 g (99.5% purity, 73.2% yield) of the product

出典と根拠

ORDレコード
ord-f67cdb9155454b4e92d2c05d19c75e4d
出典データセット
uspto-grants-2013_08
特許番号
US08519003B2

反応ノート

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