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

HRID 128318ノート

反応式

HRID 128318 の反応式
[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]

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-991296bcf9304292a33dfaab27bb379c
出典データセット
uspto-grants-1981_03
特許番号
US04259352

反応ノート

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