Nitric Acid → 2-Amino-6-methyl-5-nitropyrimidin-4-ol

HRID 1805852

반응식

HRID 1805852 반응식
[NH2:1][C:2]1[NH:7][C:6](=[O:8])[CH:5]=[C:4]([CH3:9])[N:3]=1.[N+:10]([O-])([OH:12])=[O:11].C(OCC)C>OS(O)(=O)=O>[NH2:1][C:2]1[NH:7][C:6](=[O:8])[C:5]([N+:10]([O-:12])=[O:11])=[C:4]([CH3:9])[N:3]=1

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 3283Diethyl EtherHCID 1354020552-Amino-6-methylpyrimidin-4-one

생성물 1

HCID 1354603042-Amino-6-methyl-5-nitropyrimidin-4-ol수율 81%

시약·촉매·용매 1

HCID 1118Sulfuric Acid용매

실험 절차

To a mixture of 2-amino-6-methylpyrimidin-4(3H)-one (50 g, 0.4 mol) in 250 mL of H2SO4 at 0° C. was added 40 mL of HNO3 with an additional funnel. After being stirred at room temperature for 3 h, the reaction mixture was slowly poured into 3.6 L of diethyl ether and stirred for 15 min. Decant the ether solution and added 1.0 L of ethyl acetate to the solid and stirred for 10 h. The solid (54.8 g, 81% yield) was filtered and used for next step without any further purification.

후처리

  1. stirringstirred for 15 min
  2. customDecant the ether solution
  3. additionadded 1.0 L of ethyl acetate to the solid
  4. stirringstirred for 10 h

출처 및 근거

ORD 기록
ord-c461e21874284712b32a5a08228fdcc1
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08354532B2

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