Sodium Hydroxide → 1-(2-Amino-1-ethyl)-4-(1,4-benzodioxan-5-yl)piperazine

HRID 1290781

反応式

HRID 1290781 の反応式
[Cl-].[Al+3].[Li+].[Cl-].[Cl-].[Cl-].[Cl-].[Al+3].[Cl-].[Cl-].[O:11]1[C:16]2[CH:17]=[CH:18][CH:19]=[C:20]([N:21]3[CH2:26][CH2:25][N:24]([CH2:27][C:28]#[N:29])[CH2:23][CH2:22]3)[C:15]=2[O:14][CH2:13][CH2:12]1.[OH-].[Na+]>CCOCC.O1CCCC1.C(Cl)Cl>[NH2:29][CH2:28][CH2:27][N:24]1[CH2:23][CH2:22][N:21]([C:20]2[C:15]3[O:14][CH2:13][CH2:12][O:11][C:16]=3[CH:17]=[CH:18][CH:19]=2)[CH2:26][CH2:25]1

参加物

8

反応物 4

HCID 14798Sodium HydroxideHCID 166981Aluminum;lithium;tetrachlorideHCID 6451240Aluminum(III) ChlorideHCID 10611289HCID 10611289、化合物

生成物 1

HCID 105876411-(2-Amino-1-ethyl)-4-(1,4-benzodioxan-5-yl)piperazine収率 95.3%

試薬・触媒・溶媒 3

HCID 3283Diethyl Ether溶媒2 回HCID 6344Dichloromethane溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

A suspension of lithium aluminium chloride (8.2 g) in dry ether (170 ml) was treated dropwise with a solution of aluminium chloride (8.2 g) in ether (170 ml) under cooling. After stirring for half an hour at room temperature a solution of 1-(1,4-benzodioxan-5-yl)-4-cyanomethylpiperazine (9.4 g) in dry tetrahydrofuran (250 ml) was added dropwise at 15° C. After reflux for 1.5 h the mixture was cooled and conc. sodium hydroxide solution (40 ml) was added dropwise. Filtration and removal of solvent in vacuo gave an oil which was dissolved in methylene chloride and dried over magnesium sulfate. Removal of solvent in vacuo gave 1-(2-amino-1-ethyl)-4-(1,4-benzodioxan-5-yl)piperazine (9.1 g) as a viscous oil.

後処理

  1. temperatureunder cooling
  2. additionwas added dropwise at 15° C
  3. temperatureAfter reflux for 1.5 h the mixture
  4. temperaturewas cooled
  5. filtrationFiltration and removal of solvent in vacuo
  6. customgave an oil which
  7. dry with materialdried over magnesium sulfate
  8. customRemoval of solvent in vacuo

出典と根拠

ORDレコード
ord-f57bbf6bbd734e9ea6ce8740571c0f2c
出典データセット
uspto-grants-1998_05
特許番号
US05753661

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