Trimethyl orthoformate → 3-Chloro-2-(4-chloro-3-dimethoxymethylphenyl)-5-trifluoromethylpyridine

HRID 1957260ノート

反応式

HRID 1957260 の反応式
[CH:1](OC)([O:4][CH3:5])[O:2][CH3:3].O.[O-2].[O-2].[O-2].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.[Al+3].[Al+3].[Cl:26][C:27]1[C:28]([C:37]2[CH:42]=[CH:41][C:40]([Cl:43])=[C:39](C=O)[CH:38]=2)=[N:29][CH:30]=[C:31]([C:33]([F:36])([F:35])[F:34])[CH:32]=1>ClCCl>[Cl:26][C:27]1[C:28]([C:37]2[CH:42]=[CH:41][C:40]([Cl:43])=[C:39]([CH:1]([O:4][CH3:5])[O:2][CH3:3])[CH:38]=2)=[N:29][CH:30]=[C:31]([C:33]([F:35])([F:36])[F:34])[CH:32]=1

参加物

5

反応物 3

HCID 9005Trimethyl orthoformateHCID 186929322-Chloro-5-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]benzaldehydeHCID 71586775Bentonite

生成物 1

HCID 190687453-Chloro-2-(4-chloro-3-dimethoxymethylphenyl)-5-trifluoromethylpyridine

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

50 ml of trimethyl orthoformate were added to 40.0 g of montmorillonite K-10 in 250 ml of anhydrous dichloromethane, after which a solution of 20.0 g of 3-chloro-2-(4-chloro-3-formylphenyl)-5-trifluoromethylpyridine in 50 ml of dichloromethane was added dropwise while stirring and cooling in ice. After stirring at 23° C. for 20 hours, the clay was removed and thoroughly washed with dichloromethane. The dichloromethane phase was concentrated. The residue was purified by chromatography on silica gel with cyclohexane/ethyl acetate (10:1). Yield: 22.1 g (96%) of a colorless oil.

後処理

  1. temperaturecooling in ice
  2. stirringAfter stirring at 23° C. for 20 hours
  3. customthe clay was removed
  4. washthoroughly washed with dichloromethane
  5. concentrationThe dichloromethane phase was concentrated
  6. customThe residue was purified by chromatography on silica gel with cyclohexane/ethyl acetate (10:1)

出典と根拠

ORDレコード
ord-0ffccac45b144b839e75b0fdf07c86d6
出典データセット
uspto-grants-1998_07
特許番号
US05783522

反応ノート

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