Methylurea → 1,6-Dimethyluracil

HRID 60339

반응식

HRID 60339 반응식
[CH3:1][NH:2][C:3]([NH2:5])=[O:4].[CH2:6]=[C:7]1[O:10][C:9](=O)[CH2:8]1>CO>[CH3:1][N:2]1[C:7]([CH3:6])=[CH:8][C:9](=[O:10])[NH:5][C:3]1=[O:4]

참가 물질

4

반응물 2

HCID 11719MethylureaHCID 12661Diketene

생성물 1

HCID 106068181,6-Dimethyluracil수율 18%

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 1-methylurea (30 g, 0.356 mol) in 4-methyleneoxetan-2-one (26.4 g, 0.356 mol) was heated at 100° C. for 18 h, cooled to RT then diluted with MeOH (50 mL). The reaction was filtered and the filtered solid was washed with MeOH (20 mL) and dried to give 1,6-dimethylpyrimidine-2,4(1H,3H)-dione (9 g, 18% yield) as a white solid. 1H NMR (CDCl3) δ: 8.33 (s, 1H), 5.58 (s, 1H), 3.38 (s, 3H), 2.26 (s, 3H). LCMS: MH+ 141 and TR=0.368 min. Used without further purification.

후처리

  1. filtrationThe reaction was filtered
  2. washthe filtered solid was washed with MeOH (20 mL)
  3. customdried

출처 및 근거

ORD 기록
ord-3676721470164f839a71b8ed5c811bf2
출처 데이터셋
uspto-grants-2016_09
특허 번호
US09440983B2

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