Hydrochloric Acid → HCID 69103555、化合物

HRID 2217248ノート

反応式

HRID 2217248 の反応式
[C:1]([C:4]1[N:9]=[C:8]([C:10]2[CH:11]=[CH:12][C:13](=[O:19])[N:14]([CH:16]([CH3:18])[CH3:17])[CH:15]=2)[C:7]([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)=[N:6][C:5]=1[NH2:26])(=[O:3])[CH3:2].[BH4-].[Na+].Cl.O>C1COCC1.CO.CCOC(C)=O>[NH2:26][C:5]1[N:6]=[C:7]([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[C:8]([C:10]2[CH:11]=[CH:12][C:13](=[O:19])[N:14]([CH:16]([CH3:17])[CH3:18])[CH:15]=2)=[N:9][C:4]=1[CH:1]([OH:3])[CH3:2]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 4311764Sodium borohydrideHCID 69103232HCID 69103232、化合物

生成物 1

HCID 69103555HCID 69103555、化合物収率 19.4%

試薬・触媒・溶媒 2

HCID 8857Ethyl Acetate溶媒HCID 21899815MeOH tetrahydrofuran溶媒

実験手順

To a solution of 5-(6-acetyl-5-amino-3-phenyl-2-pyrazinyl)-1-isopropyl-2(1H)-pyridone (82 mg) in THF-MeOH (1:1, 2.0 ml), was added sodium borohydride (8.9 mg). The mixture was stirred st room temperature for 4 hours. 1N HCl (0.05 ml) was poured into the mixtre. Water and EtOAc were poured into the mixture and the organic layer was separated, washed with water and brine, and dried over MgSO4. The solvent was removed under reduced pressure. The residue was purified by column chromatography. The desired product was recrystallized from EtOH and dried in vacuo to give 5-[5-amino-6-(1-hydroxyethyl)-3-phenyl-2-pyrazinyl]-1-isopropyl-2(1H)-pyridone (16 mg).

後処理

  1. customthe organic layer was separated
  2. washwashed with water and brine
  3. dry with materialdried over MgSO4
  4. customThe solvent was removed under reduced pressure
  5. customThe residue was purified by column chromatography
  6. customThe desired product was recrystallized from EtOH
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-fbe59a2f466b4fd9ab317aa711a07020
出典データセット
uspto-grants-2008_08
特許番号
US07407961B2

反応ノート

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