Cyclohexylamine → HCID 178471915, 화합물

HRID 963401노트

반응식

HRID 963401 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

HCID 178471915HCID 178471915, 화합물수율 55%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-274eff2ed84a44fe97f498e076a1e225
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05763450

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