Trifluoroiodomethane → Ethyl 3-chloro-5-trifluoromethyl-4-cyclohexylphenylglyoxylate

HRID 26557

反応式

HRID 26557 の反応式
Br[C:2]1[CH:3]=[C:4]([C:15](=[O:21])[C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH:5]=[C:6]([Cl:14])[C:7]=1[CH:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1.[F:22][C:23](I)([F:25])[F:24]>[Cu].CN(C)C=O>[Cl:14][C:6]1[CH:5]=[C:4]([C:15](=[O:21])[C:16]([O:18][CH2:19][CH3:20])=[O:17])[CH:3]=[C:2]([C:23]([F:25])([F:24])[F:22])[C:7]=1[CH:8]1[CH2:13][CH2:12][CH2:11][CH2:10][CH2:9]1

参加物

5

反応物 2

HCID 16843TrifluoroiodomethaneHCID 20515177Ethyl 3-bromo-5-chloro-4-cyclohexylphenylglyoxylate

生成物 1

HCID 20515171Ethyl 3-chloro-5-trifluoromethyl-4-cyclohexylphenylglyoxylate

試薬・触媒・溶媒 2

HCID 23978Copper触媒HCID 6228Dimethylformamide溶媒

反応条件

温度
140 °C

実験手順

To a solution of 0.01 moles of ethyl 3-bromo-5-chloro-4-cyclohexylphenylglyoxylate in 50 ml. of dimethylformamide is added 0.15 moles of trifluoromethyl iodide and 0.02 g. of copper powder. The reaction is shaken in a sealed tube for 5 hours at 140° C., cooled, filtered and evaporated in vacuo. 200 ml. of water is added to the residue and extracted with ether. The ether extract is dried, evaporated to dryness and distilled to obtain ethyl 3-chloro-5-trifluoromethyl-4-cyclohexylphenylglyoxylate.

後処理

  1. temperaturecooled
  2. filtrationfiltered
  3. customevaporated in vacuo
  4. additionof water is added to the residue
  5. extractionextracted with ether
  6. extractionThe ether extract
  7. customis dried
  8. customevaporated to dryness
  9. distillationdistilled

出典と根拠

ORDレコード
ord-db4c40927b254853a781b32f0fa78a9d
出典データセット
uspto-grants-1979_04
特許番号
US04150148

関連ノート

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