18-Crown-6 → HCID 15452060、化合物

HRID 1005487ノート

反応式

HRID 1005487 の反応式
Cl[C:2]1[C:9]([Cl:10])=[CH:8][CH:7]=[C:6]([C:11]([F:14])([F:13])[F:12])[C:3]=1[C:4]#[N:5].[F-:15].[K+].C1OCCOCCOCCOCCOCCOC1>CN(C)C=O>[Cl:10][C:9]1[C:2]([F:15])=[C:3]([C:6]([C:11]([F:14])([F:13])[F:12])=[CH:7][CH:8]=1)[C:4]#[N:5]

参加物

5

反応物 3

HCID 2855718-Crown-6HCID 522689Potassium FluorideHCID 109775462,3-Dichloro-6-(trifluoromethyl)benzonitrile

生成物 1

HCID 15452060HCID 15452060、化合物収率 72.7%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

To a solution of 0.96 g of 2,3-dichloro-6-trifluoromethylbenzonitrile in 7 ml of N,N-dimethylformamide was added 0.46 g of spray-dried potassium fluoride and 0.1 g of 18-crown-6-ether and the mixture was stirred for 6 hours at 100° C. under a nitrogen atmosphere. After cooling, the reaction mixture was poured into ice water and extracted with ethyl acetate. The organic layer was washed with saturated saline solution and dried over anhydrous magnesium sulfate. After distilling the solvent under reduced pressure, the crude product obtained was purified by using silica gel column chromatography to obtain 0.65 g of the title compound(mp. 43-44° C.).

後処理

  1. temperatureAfter cooling
  2. extractionextracted with ethyl acetate
  3. washThe organic layer was washed with saturated saline solution
  4. dry with materialdried over anhydrous magnesium sulfate
  5. distillationAfter distilling the solvent under reduced pressure
  6. customthe crude product obtained
  7. customwas purified

出典と根拠

ORDレコード
ord-9cbea0cc61ff4c699ec7bf5d529e5133
出典データセット
uspto-grants-2000_04
特許番号
US06054605

反応ノート

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