Tin tetrachloride → HCID 44139769, 화합물

HRID 1896984노트

반응식

HRID 1896984 반응식
[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

참가 물질

6

반응물 3

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

생성물 1

HCID 44139769HCID 44139769, 화합물수율 73.2%

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f67cdb9155454b4e92d2c05d19c75e4d
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08519003B2

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