Piperazine → N-(3-benzhydroxypropyl)piperazine

HRID 565633ノート

反応式

HRID 565633 の反応式
[NH:1]1[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]1.[C:7]1([CH:13]([C:19]2[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=2)[O:14][CH2:15][CH2:16][CH2:17]Br)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1>C(O)C.[Na+].[Cl-]>[C:19]1([CH:13]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)[O:14][CH2:15][CH2:16][CH2:17][N:1]2[CH2:6][CH2:5][NH:4][CH2:3][CH2:2]2)[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1

参加物

5

反応物 2

HCID 4837PiperazineHCID 143063671-(Diphenylmethoxy)-3-bromopropane

生成物 1

HCID 22110970N-(3-benzhydroxypropyl)piperazine収率 99.7%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒2 回HCID 5234Sodium Chloride溶媒

反応条件

温度
70 °C

実験手順

In 20 mL of ethanol was dissolved 20 g of piperazine with heating. Then, a solution of 3-(diphenylmethoxy)propyl bromide (7.0 g) in ethanol (20 mL) was added dropwise and the mixture was stirred at 70° C. for 1 hour. This reaction mixture was diluted with saturated aqueous NaCl and extracted with chloroform. The extract was washed with saturated aqueous NaCl to remove the starting material piperazine, dried over MgSO4, and concentrated under reduced pressure to provide 7.1 g of the title compound. Yield 99%. This product was not further purified but directly submitted to the next reaction.

後処理

  1. temperaturewith heating
  2. extractionextracted with chloroform
  3. washThe extract was washed with saturated aqueous NaCl
  4. customto remove the starting material piperazine
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-546818fe66f54360b2ea26b4243be733
出典データセット
uspto-grants-2001_01
特許番号
US06172085B2

反応ノート

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