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

HRID 2045816ノート

反応式

HRID 2045816 の反応式
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]

参加物

3

反応物 2

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

生成物 1

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

反応条件

温度
145 °C

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-a987bff9d5e3414c885614ff03dc2139
出典データセット
uspto-grants-2013_11
特許番号
US08592400B2

反応ノート

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