Methyl 6-amino-5-nitropyridine-3-carboxylate → Methyl 5,6-diaminopyridine-3-carboxylate

HRID 854095노트

반응식

HRID 854095 반응식
[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:9]=[C:8]([N+:10]([O-])=O)[C:7]([NH2:13])=[N:6][CH:5]=1>CO.[Ni]>[CH3:1][O:2][C:3](=[O:14])[C:4]1[CH:9]=[C:8]([NH2:10])[C:7]([NH2:13])=[N:6][CH:5]=1

참가 물질

4

반응물 1

HCID 13768248Methyl 6-amino-5-nitropyridine-3-carboxylate

생성물 1

HCID 9920476Methyl 5,6-diaminopyridine-3-carboxylate수율 76%

시약·촉매·용매 2

HCID 935Nickel촉매HCID 887Methanol용매

반응 조건

온도
80 °C

실험 절차

To a suspension of 6-Amino-5-nitro-nicotinic acid methyl ester (3) (5 g, 25 mmol) in MeOH (150 ml) was added Raney Ni. The mixture was vacuum purged with H2 5 times and heated at 80° C. under H2 atmosphere for 4 h. The solution was filtered through celite and concentrated in vacuo to give the product as a brown solid (3.2 g, 19 mmol, 76%) that was used without further purification. TLC of the product in DCM/MeOH (19:1) indicated a more polar spot at Rf=0.026.

후처리

  1. custompurged with H2 5 times
  2. filtrationThe solution was filtered through celite and
  3. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-e13450cda6314389bd2b3de44eb0b45b
출처 데이터셋
uspto-grants-2007_08
특허 번호
US07256287B2

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