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

HRID 370283ノート

反応式

HRID 370283 の反応式
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]

参加物

8

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 3

HCID 4875Potassium Iodide触媒HCID 1140Toluene溶媒HCID 3776Isopropanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-b24ca0e6cd364448a79b8afced73a8f9
出典データセット
uspto-grants-2000_10
特許番号
US06140501

反応ノート

読み込み中…