Methane → HCID 178477337、化合物

HRID 2287751ノート

反応式

HRID 2287751 の反応式
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

参加物

6

反応物 4

HCID 297MethaneHCID 1049Pyridine2 回HCID 14817Phosphorus sulfide (P2S5)HCID 135424359NSC403089

生成物 1

HCID 178477337HCID 178477337、化合物収率 95.9%

試薬・触媒・溶媒 1

HCID 14798Sodium Hydroxide溶媒

実験手順

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).

後処理

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

出典と根拠

ORDレコード
ord-eb7e8e8741ed42509c9bfd9bf8453198
出典データセット
uspto-grants-2000_07
特許番号
US06084095

反応ノート

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