2,4-Diamino-6-ethoxypyrimidine → 6-Ethoxy-5-nitrosopyrimidine-2,4-diamine

HRID 1178218노트

반응식

HRID 1178218 반응식
[NH2:1][C:2]1[N:7]=[C:6]([O:8][CH2:9][CH3:10])[CH:5]=[C:4]([NH2:11])[N:3]=1.[N:12]([O-])=[O:13].[Na+]>C(O)(=O)C.O>[N:12]([C:5]1[C:6]([O:8][CH2:9][CH3:10])=[N:7][C:2]([NH2:1])=[N:3][C:4]=1[NH2:11])=[O:13]

참가 물질

5

반응물 2

HCID 2226632,4-Diamino-6-ethoxypyrimidineHCID 23668193Sodium Nitrite

생성물 1

HCID 2272506-Ethoxy-5-nitrosopyrimidine-2,4-diamine수율 68.3%

시약·촉매·용매 2

HCID 176Acetic Acid용매HCID 962Water용매

반응 조건

온도
80 °C

실험 절차

To a solution of the compound of example 54 (6.13 g, 39.8 mmoles) in 20% aqueous acetic acid (57 ml) was added dropwise a solution of NaNO2 (3.29 g) in water (13 ml) at 80° C. A pink precipitate was formed which was stirred at 80° C. for an additional 2 hours. The reaction mixture was cooled down in the refrigerator overnight and the resulting precipitate was filtered off, yielding the title compound as a pink powder (4.98 g, yield 68%). Spectral data are identical with those described e.g. by W. Pfleiderer et al. in Chem. Ber. (1961) 94, 12.

후처리

  1. customA pink precipitate was formed which
  2. temperatureThe reaction mixture was cooled down in the refrigerator overnight
  3. filtrationthe resulting precipitate was filtered off

출처 및 근거

ORD 기록
ord-b51ac65faca143009dc86180aea0013a
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07276506B2

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