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

HRID 902054노트

반응식

HRID 902054 반응식
[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

참가 물질

7

반응물 4

HCID 14798Sodium HydroxideHCID 24436Sodium SulfateHCID 21226445Aluminium lithium hydrideHCID 69206757HCID 69206757, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매2회HCID 8028Tetrahydrofuran용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-232abf793bbc4b57b0d5e3745a447d4d
출처 데이터셋
uspto-grants-2008_04
특허 번호
US07365077B2

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