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

HRID 1290781

반응식

HRID 1290781 반응식
[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

참가 물질

8

반응물 4

HCID 14798Sodium HydroxideHCID 166981Aluminum;lithium;tetrachlorideHCID 6451240Aluminum(III) ChlorideHCID 10611289HCID 10611289, 화합물

생성물 1

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

시약·촉매·용매 3

HCID 3283Diethyl Ether용매2회HCID 6344Dichloromethane용매HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-f57bbf6bbd734e9ea6ce8740571c0f2c
출처 데이터셋
uspto-grants-1998_05
특허 번호
US05753661

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