p-Toluenesulfonic acid → 1-Dimethoxymethyl-2-fluoro-4-trifluoromethyl-benzene

HRID 456554

反応式

HRID 456554 の反応式
[F:1][C:2]1[CH:9]=[C:8]([C:10]([F:13])([F:12])[F:11])[CH:7]=[CH:6][C:3]=1C=O.[CH:14](OC)([O:17][CH3:18])[O:15][CH3:16].C1(C)C=CC(S(O)(=O)=O)=CC=1.C([O-])([O-])=O.[Na+].[Na+]>>[CH3:16][O:15][CH:14]([O:17][CH3:18])[C:3]1[CH:6]=[CH:7][C:8]([C:10]([F:13])([F:12])[F:11])=[CH:9][C:2]=1[F:1]

参加物

5

反応物 4

HCID 6101p-Toluenesulfonic acidHCID 9005Trimethyl orthoformateHCID 10340Sodium CarbonateHCID 5229292-Fluoro-4-(trifluoromethyl)benzaldehyde

生成物 1

HCID 231124321-Dimethoxymethyl-2-fluoro-4-trifluoromethyl-benzene収率 98%

実験手順

A solution of 2-fluoro-4-trifluoromethylbenzaldehyde (10.0 g, 52.0 mmol), trimethyl orthoformate (55.0 g, 520 mmol) and a catalytic amount of p-toluene sulfonic acid (5 mol %) was stirred at room temperature for 24 hours. The resulting solution was saturated with the addition of solid Na2CO3 and stirred for 15 minutes. The mixture was then filtered and the solution was evaporated. The residue was diluted with ether and evaporated yielding 12.1 g (98%) of the desired product as an oil.

後処理

  1. filtrationThe mixture was then filtered
  2. customthe solution was evaporated
  3. additionThe residue was diluted with ether
  4. customevaporated

出典と根拠

ORDレコード
ord-498c52f8ffc045d89e1e78af52efdcf6
出典データセット
uspto-grants-2007_03
特許番号
US07186724B2

関連ノート

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