Methane → HCID 178477337, 화합물

HRID 2256182노트

반응식

HRID 2256182 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 (0.5M, 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-68aa0bb5d3d64736840f919873cfa18c
출처 데이터셋
uspto-grants-1997_08
특허 번호
US05654307

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