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

HRID 428377

반응식

HRID 428377 반응식
[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]

참가 물질

3

반응물 2

HCID 4837PiperazineHCID 867575721,4-Benzodioxan 2-ethylcarboxylate

생성물 1

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

반응 조건

온도
110 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-3c3d3f1904a748bd821cb7e2c09615ab
출처 데이터셋
uspto-grants-2001_11
특허 번호
US06313294B1

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