Sodium Hydroxide → 1-(1-Benzyl-4-methylpiperazin-2-yl)methanamine

HRID 902054ノート

反応式

HRID 902054 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH2:7]([N:14]1[CH2:19][CH2:18][N:17]([C:20](OC(C)(C)C)=O)[CH2:16][CH:15]1[C:27](=O)[NH2:28])[C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1.[OH-].[Na+].S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1.O>[NH2:28][CH2:27][CH:15]1[CH2:16][N:17]([CH3:20])[CH2:18][CH2:19][N:14]1[CH2:7][C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1

参加物

7

反応物 4

HCID 14798Sodium HydroxideHCID 24436Sodium SulfateHCID 21226445Aluminium lithium hydrideHCID 69206757HCID 69206757、化合物

生成物 1

HCID 117756161-(1-Benzyl-4-methylpiperazin-2-yl)methanamine収率 100%

試薬・触媒・溶媒 2

HCID 962Water溶媒2 回HCID 8028Tetrahydrofuran溶媒2 回

実験手順

1M Lithium aluminium hydride in tetrahydrofuran (112 ml, 0.112 mol) was added dropwise to a stirred solution of (RS)-1-benzyl-4-(tert-butyloxycarbonyl)-2-carbamoylpiperazine (D1) (15 g, 0.047 mol) in anhydrous tetrahydrofuran (300 ml) at room temperature under argon. On complete addition the reaction mixture was stirred at room temperature for 0.5 h, then at reflux for a further 1.5 h. The mixture was cooled to room temperature and treated sequentially with water (19.5 ml), 2N sodium hydroxide (22.5 ml) and water (19.5 ml) dropwise. Sodium sulphate was added and the resultant stirred for 0.3 h, filtered and the filtrate evaporated in vacuo to give the title compound (10.3 g, 100%).

後処理

  1. additionOn complete addition the reaction mixture
  2. temperatureat reflux for a further 1.5 h
  3. temperatureThe mixture was cooled to room temperature
  4. stirringthe resultant stirred for 0.3 h
  5. filtrationfiltered
  6. customthe filtrate evaporated in vacuo

出典と根拠

ORDレコード
ord-232abf793bbc4b57b0d5e3745a447d4d
出典データセット
uspto-grants-2008_04
特許番号
US07365077B2

反応ノート

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