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HCID 86603473、化合物 → HCID 67147606、化合物

HRID 2219059
ノート
印刷プレビュー

反応式

HRID 2219059 の反応式
[F:1][C:2]1[CH:27]=[CH:26][C:5]([CH2:6][NH:7][C:8]([C:10]2[N:11]=[C:12]3[CH2:21][CH:20]([N:22](OC)[CH3:23])[CH2:19][CH2:18][N:13]3[C:14](=[O:17])[C:15]=2[OH:16])=[O:9])=[CH:4][CH:3]=1>C(O)(=O)C.O.[Zn]>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:6][NH:7][C:8]([C:10]2[N:11]=[C:12]3[CH2:21][CH:20]([NH:22][CH3:23])[CH2:19][CH2:18][N:13]3[C:14](=[O:17])[C:15]=2[OH:16])=[O:9])=[CH:26][CH:27]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 1

HCID 86603473HCID 86603473、化合物

生成物 1

HCID 67147606HCID 67147606、化合物

試薬・触媒・溶媒 2

HCID 23994Zinc触媒2 回HCID 21899381Acetic acid--water (1/1)溶媒

実験手順

To a solution of crude N-(4-fluorobenzyl)-3-hydroxy-8-[methoxy(methyl)amino]-4-oxo-6,7,8,9-tetrahydro-4H-pyrido[1,2-a]pyrimidine-2-carboxamide in acetic acid/water (2:1) was added zinc dust (300% in weight). The mixture was stirred at room temperature and after 1.5 h further zinc dust (300% in weight) was added. After 24 h zinc was filtered off and the filtrate was concentrated to dryness. The residue was dissolved in methanol and applied on a SCX resin cartridge. The cartridge was washed with water and methanol and then eluted with ammonia in methanol (2N). The eluent was concentrated to dryness. The crude product so obtained was used in the subsequent step without further purification.

後処理

  1. additionwas added
  2. filtrationAfter 24 h zinc was filtered off
  3. concentrationthe filtrate was concentrated to dryness
  4. dissolutionThe residue was dissolved in methanol
  5. washThe cartridge was washed with water and methanol
  6. washeluted with ammonia in methanol (2N)
  7. concentrationThe eluent was concentrated to dryness

出典と根拠

ORDレコード
ord-5a169befa79c4a7cab4a549ce1d87702
出典データセット
uspto-grants-2008_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07414045B2

反応ノート

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