Cyclohexylamine → HCID 178471915、化合物

HRID 963401ノート

反応式

HRID 963401 の反応式
[Cl:1][C:2]1[CH:19]=[C:18]([I:20])[CH:17]=[CH:16][C:3]=1[C:4]([C:6](=[CH:12]OCC)[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5].[CH:21]1([NH2:27])[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1>C(Cl)Cl>[Cl:1][C:2]1[CH:19]=[C:18]([I:20])[CH:17]=[CH:16][C:3]=1[C:4]([C:6](=[CH:12][NH:27][CH:21]1[CH2:26][CH2:25][CH2:24][CH2:23][CH2:22]1)[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:5]

参加物

4

反応物 2

HCID 7965CyclohexylamineHCID 53916769Ethyl 2-(2-chloro-4-iodo-benzoyl)-3-ethoxy-acrylate

生成物 1

HCID 178471915HCID 178471915、化合物収率 55%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

mf) A solution of 31.18 g of ethyl 2-(2-chloro-4-iodo-benzoyl)-3-ethoxy-acrylate in 500 ml of methylene chloride is treated dropwise with 7.95 g of cyclohexylamine while cooling with ice and stirring. After 6 hrs. at room temperature the reaction mixture is concentrated and, for crystallization, the residue is stirred with 200 ml of hexane. The precipitate is filtered off under suction, washed with 100 ml of hexane and dried. 19.2 g (55%) of ethyl 2-(2-chloro-4-iodo-benzoyl)-3-cyclohexylamino-acrylate are obtained as a colourless solid. M.p. 154°-156° C.

後処理

  1. temperaturewhile cooling with ice
  2. concentrationat room temperature the reaction mixture is concentrated and, for crystallization
  3. stirringthe residue is stirred with 200 ml of hexane
  4. filtrationThe precipitate is filtered off under suction
  5. washwashed with 100 ml of hexane
  6. customdried

出典と根拠

ORDレコード
ord-274eff2ed84a44fe97f498e076a1e225
出典データセット
uspto-grants-1998_06
特許番号
US05763450

反応ノート

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