Diethyl Sulfate → HCID 23324656, 화합물

HRID 1380828노트

반응식

HRID 1380828 반응식
[Cl:1][CH2:2][C:3]1[N:8]=[C:7]([CH3:9])[N:6]=[C:5]([OH:10])[CH:4]=1.S(OCC)(O[CH2:15][CH3:16])(=O)=O.C(=O)([O-])[O-].[K+].[K+]>CC(C)=O>[CH2:15]([O:10][C:5]1[N:6]=[C:7]([CH3:9])[N:8]=[C:3]([CH2:2][Cl:1])[CH:4]=1)[CH3:16]

참가 물질

5

반응물 3

HCID 6163Diethyl SulfateHCID 11430Potassium CarbonateHCID 178433451HCID 178433451, 화합물

생성물 1

HCID 23324656HCID 23324656, 화합물

시약·촉매·용매 1

HCID 180Acetone용매

실험 절차

15.8 g (0.1 mol) of 6-chloromethyl-4-hydroxy-2-methyl-pyrimidine, 13 ml (0.1 mol) of diethyl sulphate and 27.6 g (0.2 mol) of potassium carbonate are heated at reflux in 500 ml of acetone for 6 hours. The mixture is then filtered and the filtrate is concentrated to dryness. The residue is taken up in 200 ml of methylene chloride and the methylene chloride solution is washed once with 50 ml of 2N sodium hydroxide and twice with 50 ml of semi-saturated sodium chloride solution, dried over anhydrous sodium sulphate and evaporated under reduced pressure. The residual oil is distilled at 47° C./0.07 mmHg, whereupon the distillate becomes solid. There is obtained 6-ethoxy-4-chloromethyl-2-methyl-pyrimidine, m.p. 29° C.

후처리

  1. filtrationThe mixture is then filtered
  2. concentrationthe filtrate is concentrated to dryness
  3. washthe methylene chloride solution is washed once with 50 ml of 2N sodium hydroxide and twice with 50 ml of semi-saturated sodium chloride solution
  4. dry with materialdried over anhydrous sodium sulphate
  5. customevaporated under reduced pressure
  6. distillationThe residual oil is distilled at 47° C./0.07 mmHg

출처 및 근거

ORD 기록
ord-86e51d68990f4b8b84e09f5a37e8864b
출처 데이터셋
uspto-grants-1986_04
특허 번호
US04584295

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