Potassium Carbonate → Ethyl 3-[4-(2-allylcyclohexylamino)phenyl]propionate

HRID 128318노트

반응식

HRID 128318 반응식
[NH2:1][C:2]1[CH:14]=[CH:13][C:5]([CH2:6][CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:4][CH:3]=1.CS(O[CH:20]1[CH2:25][CH2:24][CH2:23][CH2:22][CH:21]1[CH2:26][CH:27]=[CH2:28])(=O)=O.C(=O)([O-])[O-].[K+].[K+].CN(C)P(N(C)C)(N(C)C)=O>O>[CH2:26]([CH:21]1[CH2:22][CH2:23][CH2:24][CH2:25][CH:20]1[NH:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][CH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])=[CH:13][CH:14]=1)[CH:27]=[CH2:28]

참가 물질

6

반응물 4

HCID 11430Potassium CarbonateHCID 12679HexamethylphosphoramideHCID 10442595Ethyl 3-(4-aminophenyl)propanoateHCID 204988971-Methanesulfonyloxy-2-allylcyclohexane

생성물 1

HCID 20498965Ethyl 3-[4-(2-allylcyclohexylamino)phenyl]propionate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 5.0 g. of ethyl 4-aminohydrocinnamate, 10.0 g. of 1-methanesulfonyloxy-2-allylcyclohexane (prepared by the method of Example 189), 4.2 g. of anhydrous powdered potassium carbonate and 40 ml. hexamethylphosphoramide is heated to 80 for 17 hours. The mixture is then cooled, diluted with water and extracted with ethyl ether. The ether extracts are washed with water, dried and evaporated. The residue is recrystallized from ethanol yielding the title compound as white crystals.

후처리

  1. additionA mixture of 5.0 g
  2. temperatureThe mixture is then cooled
  3. extractionextracted with ethyl ether
  4. washThe ether extracts are washed with water
  5. customdried
  6. customevaporated
  7. customThe residue is recrystallized from ethanol yielding the title compound as white crystals

출처 및 근거

ORD 기록
ord-991296bcf9304292a33dfaab27bb379c
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04259352

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