Water → Ethyl 4-(2-carbamoylmethoxyethyl)piperazine-1-carboxylate

HRID 1383753노트

반응식

HRID 1383753 반응식
Cl[CH2:2][CH2:3][O:4][CH2:5][C:6]([NH2:8])=[O:7].[N:9]1([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1.C(=O)([O-])[O-].[Na+].[Na+].O>C1(C)C=CC=CC=1.[I-].[K+].C(O)(C)C>[C:6]([CH2:5][O:4][CH2:3][CH2:2][N:12]1[CH2:11][CH2:10][N:9]([C:15]([O:17][CH2:18][CH3:19])=[O:16])[CH2:14][CH2:13]1)(=[O:7])[NH2:8]

참가 물질

8

반응물 4

HCID 962WaterHCID 84311-Piperazinecarboxylic acid, ethyl esterHCID 10340Sodium CarbonateHCID 110189312-(2-Chloroethoxy)acetamide

생성물 1

HCID 21188378Ethyl 4-(2-carbamoylmethoxyethyl)piperazine-1-carboxylate수율 82.3%

시약·촉매·용매 3

HCID 4875Potassium Iodide촉매HCID 1140Toluene용매HCID 3776Isopropanol용매

실험 절차

15.13 g of (2-chloroethoxy)acetamide (0.11 mol), 14.6 ml of ethyl piperazine carboxylate (0.1 mol), 23.3 g of sodium carbonate (0.22 mol) and 1.0 g of potassium iodide in 25 ml of toluene are introduced into a round-bottomed flask fitted with a water-cooled condenser and a mechanical stirrer. The mixture is heated at the reflux temperature for 4 hours and is allowed to cool to room temperature. The reaction is continued, still with stirring, for a further 16 hours. 100 ml of isopropanol are added and the solid materials formed are filtered off. The solvent is evaporated from the filtrate under reduced pressure to dryness. The product obtained after evaporation of the solvents is recrystallized from toluene. 21.35 g of ethyl 4-(2-carbamoylmethoxyethyl)piperazine-1-carboxylate are obtained. Yield: 82%. Mass spectrum: 260 (MH+), 214 (M+−OEt).

후처리

  1. temperaturecooled condenser and a mechanical stirrer
  2. temperatureThe mixture is heated at the reflux temperature for 4 hours
  3. customthe solid materials formed
  4. filtrationare filtered off
  5. customThe solvent is evaporated from the filtrate under reduced pressure to dryness
  6. customThe product obtained
  7. customafter evaporation of the solvents
  8. customis recrystallized from toluene

출처 및 근거

ORD 기록
ord-453d91fe6e56431e8f6fb19b2bde1b77
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06255487B1

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