Acetic Acid → 4-Pyrimidinol, 6-methyl-5-propyl-

HRID 916635ノート

反応式

HRID 916635 の反応式
C[O-].[Na+].[CH:4]([NH2:6])=[NH:5].C[O:8][C:9](=O)[CH:10]([C:14](=O)[CH3:15])[CH2:11][CH2:12][CH3:13].C(O)(=O)C>CO>[CH2:11]([C:10]1[C:9](=[O:8])[NH:5][CH:4]=[N:6][C:14]=1[CH3:15])[CH2:12][CH3:13]

参加物

6

反応物 4

HCID 176Acetic AcidHCID 68047FormamidineHCID 10942334Sodium MethoxideHCID 14360044Methyl 2-acetylpentanoate

生成物 1

HCID 1355027734-Pyrimidinol, 6-methyl-5-propyl-

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

NaOMe (1.30 g, 24 mmol) is added to a stirred solution of formamidine (12 mmol) in MeOH (75 ml) at room temperature. The mixture is stirred for 15 minutes. 2-Acetyl-pentanoic acid methyl ester (10 mmol) is added and the mixture is stirred at room temperature overnight. Acetic acid (0.72 g, 12 mmol) is added and the solvent is removed in vacuo. Water (30 ml) is added to the residue and it is extracted with 2-butanone (3×30 ml). The combined extracts are washed with brine (40 ml), dried (Na2SO4) and evaporated, to provide a yellow solid (100), which is used in the next step without further purification.

後処理

  1. stirringthe mixture is stirred at room temperature overnight
  2. customthe solvent is removed in vacuo
  3. additionWater (30 ml) is added to the residue and it
  4. extractionis extracted with 2-butanone (3×30 ml)
  5. washThe combined extracts are washed with brine (40 ml)
  6. dry with materialdried (Na2SO4)
  7. customevaporated

出典と根拠

ORDレコード
ord-81e28272e9524300a4369e301ab93afd
出典データセット
uspto-grants-2007_09
特許番号
US07271170B2

反応ノート

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