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

HRID 82247

반응식

HRID 82247 반응식
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]

참가 물질

5

반응물 3

HCID 74900Diethyl allylmalonateHCID 160693Formamidine acetateHCID 10942334Sodium Methoxide

생성물 1

HCID 254215755-Allylpyrimidine-4,6-diol수율 57%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8d9eb956cc6845f2a0afad3fa487d257
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08846698B2

연결된 노트

불러오는 중…