Diethyl allylmalonate → 5-Allylpyrimidine-4,6-diol

HRID 82247

反応式

HRID 82247 の反応式
C([O:3][C:4](=O)[CH:5]([CH2:11][CH:12]=[CH2:13])[C:6](OCC)=[O:7])C.C[O-].[Na+].C(O)(=O)C.[CH:22]([NH2:24])=[NH:23]>C(O)C>[CH2:11]([C:5]1[C:6](=[O:7])[NH:24][CH:22]=[N:23][C:4]=1[OH:3])[CH:12]=[CH2:13]

参加物

5

反応物 3

HCID 74900Diethyl allylmalonateHCID 160693Formamidine acetateHCID 10942334Sodium Methoxide

生成物 1

HCID 254215755-Allylpyrimidine-4,6-diol収率 57%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-Allyl-malonic acid diethyl ester (Preparation 205, 100 g, 0.5 mol) was added dropwise to a mixture of sodium methoxide (27 g, 0.5 mol) in ethanol (1 L) at 0-5° C. and the mixture was stirred at this temperature for 10 min. Formamidine acetate (51.9 g, 0.5 mol) was added and the mixture was stirred at room temperature overnight. The solvent was removed in vacuo, and aqueous hydrochloric acid (36.5%) and water were added to adjust the pH to approximately 3 at 0-20° C. The resulting mixture was filtered to afford the title compound as a colorless solid in 57% yield, 87.12 g.

後処理

  1. stirringthe mixture was stirred at room temperature overnight
  2. customThe solvent was removed in vacuo, and aqueous hydrochloric acid (36.5%) and water
  3. additionwere added
  4. customat 0-20° C
  5. filtrationThe resulting mixture was filtered

出典と根拠

ORDレコード
ord-8d9eb956cc6845f2a0afad3fa487d257
出典データセット
uspto-grants-2014_09
特許番号
US08846698B2

関連ノート

読み込み中…