Hydrochloric Acid → 3-amino-N,N-dimethylbenzylamine

HRID 914966

반응식

HRID 914966 반응식
[CH3:1][N:2]([CH3:13])[CH2:3][C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([N+:10]([O-])=O)[CH:5]=1.Cl.Cl[Sn]Cl>CO>[CH3:13][N:2]([CH2:3][C:4]1[CH:5]=[C:6]([CH:7]=[CH:8][CH:9]=1)[NH2:10])[CH3:1]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 24479Stannous ChlorideHCID 308050Dimethyl-(3-nitrobenzyl)-amine

생성물 1

HCID 992943-amino-N,N-dimethylbenzylamine수율 49.9%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

To a solution of 11 (1.2 g, 6.67 mmol) in methanol (100 mL) were sequentially added conc. HCl (10 mL) and SnCl2 (5 g, 26.67 mmol). The reaction mixture was stirred at room temperature overnight before it was partitioned between water and EtOAc (200 mL each). The organic layer was separated and washed with water (150 mL), brine (150 mL) and dried over Na2SO4. The solids were filtered and the filtrate was concentrated on a rotavap to give 12 (500 mg).

후처리

  1. customwas partitioned between water and EtOAc (200 mL each)
  2. customThe organic layer was separated
  3. washwashed with water (150 mL), brine (150 mL)
  4. dry with materialdried over Na2SO4
  5. filtrationThe solids were filtered
  6. concentrationthe filtrate was concentrated on a rotavap

출처 및 근거

ORD 기록
ord-eec84e5c1d714d66918bd10e24a6ffeb
출처 데이터셋
uspto-grants-2007_09
특허 번호
US07265122B2

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