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tert-Butyl 4-(2-chloroethyl)piperazinecarboxylate → tert-Butyl 4-(2-(methylamino)ethyl)piperazine-1-carboxylate

HRID 856083
ノート
印刷プレビュー

反応式

HRID 856083 の反応式
Cl[CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][N:7]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH2:6][CH2:5]1.CO.[CH3:19][NH2:20]>CO>[CH3:19][NH:20][CH2:2][CH2:3][N:4]1[CH2:9][CH2:8][N:7]([C:10]([O:12][C:13]([CH3:16])([CH3:15])[CH3:14])=[O:11])[CH2:6][CH2:5]1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 22106269tert-Butyl 4-(2-chloroethyl)piperazinecarboxylateHCID 57454252Monomethylamine methanol

生成物 1

HCID 23081391tert-Butyl 4-(2-(methylamino)ethyl)piperazine-1-carboxylate収率 98%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

Tert-butyl 4-(2-chloroethyl)piperazine-1-carboxylate (3.13 g, 12.58 mmol) was dissolved in methanol (20 ml), to which 40% methylamine methanol solution (30 ml) was added, and the mixture was heated under reflux for 5 hours. The reaction mixture was concentrated under reduced pressure, and the residue was dissolved in methylene chloride. The mixture was washed with saturated sodium hydrogencarbonate aqueous solution. The organic layer was dried over magnesium sulfate, and then filtered, and the filtrate was concentrated under reduced pressure to afford tert-butyl 4-(2-methylaminoethyl)piperazine-1-carboxylate (3.0 g, yield 98%) as a pale yellow oil.

後処理

  1. additionwas added
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 5 hours
  4. concentrationThe reaction mixture was concentrated under reduced pressure
  5. dissolutionthe residue was dissolved in methylene chloride
  6. washThe mixture was washed with saturated sodium hydrogencarbonate aqueous solution
  7. dry with materialThe organic layer was dried over magnesium sulfate
  8. filtrationfiltered
  9. concentrationthe filtrate was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-706d8394160b4315bd33841d9aca6d42
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07262212B2

反応ノート

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