Methylurea → 1,6-Dimethyluracil

HRID 60339

反応式

HRID 60339 の反応式
[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]

参加物

4

反応物 2

HCID 11719MethylureaHCID 12661Diketene

生成物 1

HCID 106068181,6-Dimethyluracil収率 18%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-3676721470164f839a71b8ed5c811bf2
出典データセット
uspto-grants-2016_09
特許番号
US09440983B2

関連ノート

読み込み中…