Piperazine → N-1,4-Benzodioxane-2-carbonyl piperazine

HRID 428377

反応式

HRID 428377 の反応式
[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[O:4][CH2:3][CH2:2]1.CC[C:13]([O-:15])=O.[NH:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1>>[O:1]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:5]=2[O:4][CH2:3][CH:2]1[C:13]([N:16]1[CH2:21][CH2:20][NH:19][CH2:18][CH2:17]1)=[O:15]

参加物

3

反応物 2

HCID 4837PiperazineHCID 867575721,4-Benzodioxan 2-ethylcarboxylate

生成物 1

HCID 2735449N-1,4-Benzodioxane-2-carbonyl piperazine収率 94%

反応条件

温度
110 °C

実験手順

1,4-benzodioxan-2-ethylcarboxylate, (31.2 g, 150 -mmol) and piperazine (15.5 g, 180 mmol) were stirred under nitrogen and heated to 110° C. After 5 hours, the reaction was completed, which was confirmed by thin film chromatography. The crude product was cooled to room temperature, extracted with chloroform, washed with NaHCO3 solution and water. The organic layer was dried with anhydrous sodium sulfate, filtered to afford 34.96 g of compound 1 (94% yield).

後処理

  1. extractionextracted with chloroform
  2. washwashed with NaHCO3 solution and water
  3. dry with materialThe organic layer was dried with anhydrous sodium sulfate
  4. filtrationfiltered

出典と根拠

ORDレコード
ord-3c3d3f1904a748bd821cb7e2c09615ab
出典データセット
uspto-grants-2001_11
特許番号
US06313294B1

関連ノート

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