Methane → HCID 178477337, 화합물

HRID 1059636노트

반응식

HRID 1059636 반응식
O=[C:2]1[C:11]2[C:6](=[N:7][C:8]([S:12][CH2:13][CH3:14])=[N:9][CH:10]=2)[N:5]=[CH:4][NH:3]1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:16].N1C=CC=CC=1.C>[OH-].[Na+]>[S:16]=[C:2]1[C:11]2[C:6](=[N:7][C:8]([S:12][CH2:13][CH3:14])=[N:9][CH:10]=2)[N:5]=[CH:4][NH:3]1

참가 물질

6

반응물 4

HCID 297MethaneHCID 1049Pyridine2회HCID 14817Phosphorus sulfide (P2S5)HCID 135424359NSC403089

생성물 1

HCID 178477337HCID 178477337, 화합물수율 95.9%

시약·촉매·용매 1

HCID 14798Sodium Hydroxide용매

실험 절차

A mixture of 4-oxo-7-ethylthio-3H-pyrimido[4,5-d]pyrimidine (1.33 g, 6.7 mmol), P2S5 (1.48 g, 6.6 mmol) and pyridine (15 mL) is refluxed under N2 for 3 h. The pyridine is then stripped under reduced pressure, and the residue is dissolved in NaOH solution (0.5 M, 75 mL) and boiled with charcoal. After filtration, the filtrate is neutralized with acetic acid to generate a gold brown solid. Buchner filtration and drying in a vacuum oven affords 4-thiono-7-ethylthio-3H-pyrimido[4,5-d]pyrimidine (1.42 g, 95%). 1H NMR (DMSO) δ 9.47 (1H, s), 8.46 (1H, s), 3.20 (2H, q, J=7.3 Hz), 1.35 (3H, t, J=7.3 Hz).

후처리

  1. temperatureis refluxed under N2 for 3 h
  2. filtrationAfter filtration
  3. filtrationBuchner filtration
  4. customdrying in a vacuum oven

출처 및 근거

ORD 기록
ord-2a76675422fe4a04bbb03d96e8f50407
출처 데이터셋
uspto-grants-2003_02
특허 번호
US06521620B1

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