Water → HCID 19068959、化合物

HRID 1735114ノート

反応式

HRID 1735114 の反応式
[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]2[CH:11]=[CH:12][S:13][C:3]1=2.[F:14][C:15]([F:26])([F:25])[C:16](OC1C=CC=CN=1)=[O:17].[Al+3].[Cl-].[Cl-].[Cl-].O>ClCCCl>[CH3:1][N:2]1[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[C:4]2[C:11]([C:16](=[O:17])[C:15]([F:26])([F:25])[F:14])=[CH:12][S:13][C:3]1=2

参加物

6

反応物 4

HCID 962WaterHCID 46382142-(Trifluoroacetoxy)pyridineHCID 6451240Aluminum(III) ChlorideHCID 19068992HCID 19068992、化合物

生成物 1

HCID 19068959HCID 19068959、化合物

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

反応条件

温度
-10 °C

実験手順

A mixture of 1 g of (73) and 1.1 g of 2-trifluoromethylcarbonyloxypyridine, prepared according to the literature (Keumi, T. et. al. Chem. Lett. 5 (1990) 783-6), in 25 ml of 1,2-dichloroethane, was cooled to -10° C. with stirring. 1.5 g of AlCl3 was added over 15 minutes at this temperature, the reaction mixture was stirred at 0° C. for 4 hours, and at room temperature overnight. Water was added, the phases separated, and the organic phase dried and evaporated to dryness. Purification by column chromatography on silica gel in toluene gave the pure (74). Yield 590 mg. M.p. 138°-40° C.

後処理

  1. customprepared
  2. stirringthe reaction mixture was stirred at 0° C. for 4 hours
  3. customat room temperature
  4. customovernight
  5. customthe phases separated
  6. customthe organic phase dried
  7. customevaporated to dryness
  8. customPurification by column chromatography on silica gel in toluene

出典と根拠

ORDレコード
ord-0a2765c1086248439f7cef9063d18399
出典データセット
uspto-grants-1996_07
特許番号
US05536721

反応ノート

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