Trifluoroacetic acid → (+/-)-5-[7-Ethyl-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-yl]-1-methyl-2,4(1H,3H)-pyrimidinedione

HRID 324464

反応式

HRID 324464 の反応式
[CH3:1][N:2]1[CH:9]=[CH:8][C:6](=[O:7])[NH:5][C:3]1=[O:4].[CH2:10]([C:12]1[CH:13]=[CH:14][C:15]2[CH:25](O)[C:20]3[N:21]=[C:22]([CH3:24])[S:23][C:19]=3[CH:18]=[CH:17][C:16]=2[CH:27]=1)[CH3:11].FC(F)(F)C(O)=O>ClCCl>[CH2:10]([C:12]1[CH:13]=[CH:14][C:15]2[CH:25]([C:8]3[C:6](=[O:7])[NH:5][C:3](=[O:4])[N:2]([CH3:1])[CH:9]=3)[C:20]3[N:21]=[C:22]([CH3:24])[S:23][C:19]=3[CH:18]=[CH:17][C:16]=2[CH:27]=1)[CH3:11]

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 120091-MethyluracilHCID 70113719(+/-)-7-Ethyl-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-ol

生成物 1

HCID 70113042(+/-)-5-[7-Ethyl-2-methyl-4H-benzo[5,6]cyclohepta[1,2-d]thiazol-4-yl]-1-methyl-2,4(1H,3H)-pyrimidinedione

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

1-Methyluracil (0.064 g) was added to a solution of the product from step (xi) (0.10 g) in dichloromethane (2 ml), followed by trifluoroacetic acid (1 ml). The orange solution was stirred at room temperature for 10 minutes before the solvent was removed under reduced pressure. The residue was azeotroped twice with acetonitrile, and the crude product purified by chromatography, eluting with 0-5% methanol in ethyl acetate.

後処理

  1. customwas removed under reduced pressure
  2. customThe residue was azeotroped twice with acetonitrile
  3. customthe crude product purified by chromatography
  4. washeluting with 0-5% methanol in ethyl acetate

出典と根拠

ORDレコード
ord-f8231aed488949d49c4339c3952f52d4
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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