Ethanol → HCID 19068781、化合物

HRID 1957263ノート

反応式

HRID 1957263 の反応式
[O-:1][CH2:2][CH3:3].[Na+].[Cl:5][C:6]1[C:7]([C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[C:18]([CH:23]=O)[CH:17]=2)=[N:8][CH:9]=[C:10]([C:12]([F:15])([F:14])[F:13])[CH:11]=1.[CH2:25]([OH:27])[CH3:26]>C1(C)C=CC=CC=1>[Cl:5][C:6]1[C:7]([C:16]2[CH:21]=[CH:20][C:19]([Cl:22])=[C:18](/[CH:23]=[CH:3]/[C:2]([O:27][CH2:25][CH3:26])=[O:1])[CH:17]=2)=[N:8][CH:9]=[C:10]([C:12]([F:14])([F:15])[F:13])[CH:11]=1

参加物

5

反応物 3

HCID 702EthanolHCID 2723922Sodium ethoxideHCID 186929322-Chloro-5-[3-chloro-5-(trifluoromethyl)pyridin-2-yl]benzaldehyde

生成物 1

HCID 19068781HCID 19068781、化合物収率 71%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
20 °C

実験手順

A solution of 1.35 g of sodium ethoxide in 20 ml of anhydrous ethanol was added dropwise to 4.0 g of 3-chloro-2-(4-chloro-3-formylphenyl)-5-trifluoromethylpyridine and 2.9 g of triethyl phosphonatoacetate in 70 ml of anhydrous toluene. After stirring at about 20° C. for 44 hours, the solvent was removed. The residue was taken up in 100 ml of 10% strength hydrochloric acid and extracted three times with 100 ml of ethyl acetate each time. The combined organic phases were washed with 100 concentrated. Chromatography on silica gel with cyclohexane/ethyl acetate (10:1) resulted in 3.4 g (71%) of colorless crystals; melting point: 118°-120° C.

後処理

  1. customthe solvent was removed
  2. extractionextracted three times with 100 ml of ethyl acetate each time
  3. washThe combined organic phases were washed with 100
  4. concentrationconcentrated

出典と根拠

ORDレコード
ord-42a589cf91c6425baafb00b43ab60e9b
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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