1-Methyluracil → (+/-)-1-Methyl-5-(2-methyl-7-n-propyl-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-yl)-2,4-(1H,3H)-pyrimidinedione

HRID 324468

反応式

HRID 324468 の反応式
[CH3:1][N:2]1[CH:9]=[CH:8][C:6](=[O:7])[NH:5][C:3]1=[O:4].[CH3:10][C:11]1[S:12][C:13]2[CH:20]=[CH:19][C:18]3[CH:21]=[C:22]([CH2:25][CH2:26][CH3:27])[CH:23]=[CH:24][C:17]=3[CH:16](O)[C:14]=2[N:15]=1>C(O)(=O)C>[CH3:1][N:2]1[CH:9]=[C:8]([CH:16]2[C:14]3[N:15]=[C:11]([CH3:10])[S:12][C:13]=3[CH:20]=[CH:19][C:18]3[CH:21]=[C:22]([CH2:25][CH2:26][CH3:27])[CH:23]=[CH:24][C:17]2=3)[C:6](=[O:7])[NH:5][C:3]1=[O:4]

参加物

4

反応物 2

HCID 120091-MethyluracilHCID 70112533(+/-)-2-Methyl-7-n-propyl-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-ol

生成物 1

HCID 70115254(+/-)-1-Methyl-5-(2-methyl-7-n-propyl-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-yl)-2,4-(1H,3H)-pyrimidinedione

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A mixture of the 1-methyluracil (0.5 g) and the product from step (xi) in acetic acid (50 ml) was heated at reflux 2 h. The solvent was removed under reduced pressure and the residue partitioned between ethyl acetate/water. The organic layer collected and dried over MgSO4. The solvent evaporated and the crude product purified by flash chromatography eluting with ethyl acetate.

後処理

  1. temperatureat reflux 2 h
  2. customThe solvent was removed under reduced pressure
  3. customthe residue partitioned between ethyl acetate/water
  4. customThe organic layer collected
  5. dry with materialdried over MgSO4
  6. customThe solvent evaporated
  7. customthe crude product purified by flash chromatography
  8. washeluting with ethyl acetate

出典と根拠

ORDレコード
ord-f8bee6b99aaa4484b4d79496ff0e3701
出典データセット
uspto-grants-2001_04
特許番号
US06218376B1

関連ノート

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