Piperazine → 7-ethyl-2-piperazin-1-yl-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine

HRID 2045816노트

반응식

HRID 2045816 반응식
Cl[C:2]1[CH:3]=[N:4][C:5]2[CH2:11][CH2:10][N:9]([CH2:12][CH3:13])[CH2:8][CH2:7][C:6]=2[N:14]=1.[NH:15]1[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]1>>[CH2:12]([N:9]1[CH2:10][CH2:11][C:5]2[N:4]=[CH:3][C:2]([N:15]3[CH2:20][CH2:19][NH:18][CH2:17][CH2:16]3)=[N:14][C:6]=2[CH2:7][CH2:8]1)[CH3:13]

참가 물질

3

반응물 2

HCID 4837PiperazineHCID 580715892-chloro-7-ethyl-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine

생성물 1

HCID 580716007-ethyl-2-piperazin-1-yl-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine수율 52.6%

반응 조건

온도
145 °C

실험 절차

3 g 2-chloro-7-ethyl-6,7,8,9-tetrahydro-5H-pyrazino[2,3-d]azepine are combined with 23.3 g piperazine and the mixture is heated to 145° C. for 5 hours. Excess piperazine is distilled off and the residue is treated with dichloromethane and methanol. Any product precipitated is suction filtered and purified by chromatography (Alox, dioxane/toluene/methanol/NH4OH 50/20/20/2). 1.95 g product are obtained.

후처리

  1. distillationExcess piperazine is distilled off
  2. additionthe residue is treated with dichloromethane and methanol
  3. customAny product precipitated
  4. filtrationfiltered
  5. custompurified by chromatography (Alox, dioxane/toluene/methanol/NH4OH 50/20/20/2)

출처 및 근거

ORD 기록
ord-a987bff9d5e3414c885614ff03dc2139
출처 데이터셋
uspto-grants-2013_11
특허 번호
US08592400B2

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