1-(6-Methoxypyridin-3-yl)-2-nitro-propan-1-ol → 2-Amino-1-[6-methoxypyridin-3-yl]propan-1-ol

HRID 1661478노트

반응식

HRID 1661478 반응식
[CH3:1][O:2][C:3]1[N:8]=[CH:7][C:6]([CH:9]([OH:15])[CH:10]([N+:12]([O-])=O)[CH3:11])=[CH:5][CH:4]=1.[H][H]>CO.[Pd]>[NH2:12][CH:10]([CH3:11])[CH:9]([C:6]1[CH:7]=[N:8][C:3]([O:2][CH3:1])=[CH:4][CH:5]=1)[OH:15]

참가 물질

5

반응물 2

HCID 593397011-(6-Methoxypyridin-3-yl)-2-nitro-propan-1-olHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 597865832-Amino-1-[6-methoxypyridin-3-yl]propan-1-ol수율 24%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

1-(6-methoxypyridin-3-yl)-2-nitro-propan-1-ol (2.20 g, 10.37 mmol) was dissolved in methanol (410 mL) and hydrogenated using a H-Cube™ hydrogenation reactor (THALES nanotechnology) equipped with a cartridge of 10% Pd/C. The flow rate was set to 0.8 mL/min, temperature 80° C. and full the hydrogen production at full mode. After evaporation of the solution diastereomers can be separated on preparative HPLC (XTerrra C18, 19×50 mm) using a gradient of 5-30% acetonitrile in water (+1% NH3) gave the pure subtitle compound (448 mg, 24%).

후처리

  1. customwas set to 0.8 mL/min, temperature 80° C.
  2. customAfter evaporation of the solution diastereomers
  3. customcan be separated on preparative HPLC (XTerrra C18, 19×50 mm)

출처 및 근거

ORD 기록
ord-c3b9268e9efb4644b51ba3aa7a13f46e
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08030340B2

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