Sodium borohydride → HCID 70656222、化合物

HRID 2401309ノート

反応式

HRID 2401309 の反応式
[C:1]([C:4]1[CH:5]=[C:6]([CH:26]=[CH:27][CH:28]=1)[O:7][C:8]1[N:9]([CH2:23][CH2:24][CH3:25])[C:10](=[O:22])[C:11]2[NH:12][C:13]([CH:17]3[CH2:21][CH2:20][CH2:19][CH2:18]3)=[N:14][C:15]=2[N:16]=1)(=[O:3])[CH3:2].[BH4-].[Na+]>C(O)C>[CH:17]1([C:13]2[NH:12][C:11]3[C:10](=[O:22])[N:9]([CH2:23][CH2:24][CH3:25])[C:8]([O:7][C:6]4[CH:26]=[CH:27][CH:28]=[C:4]([CH:1]([OH:3])[CH3:2])[CH:5]=4)=[N:16][C:15]=3[N:14]=2)[CH2:21][CH2:20][CH2:19][CH2:18]1

参加物

4

反応物 2

HCID 4311764Sodium borohydrideHCID 67192531HCID 67192531、化合物

生成物 1

HCID 70656222HCID 70656222、化合物収率 85%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-(3-Acetyl-phenoxy)-8-cyclopentyl-1-propyl-1,7-dihydro-purin-6-one (0.05 g, 0.178 mmol) was taken in ethanol (2 ml). To this was added NaBH4 (0.02 mg, 0.525 mmol) at 0° C. and stirred at room temperature for 2 hours. The reaction mixture was quenched with saturated NH4Cl and solvent was concentrated under reduced pressure. Aqueous layer was extracted with ethyl acetate and organic layer was washed with brine, dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by preparative HPLC using 1% methanol in dichloromethane as solvent system to give the product as off white solid (0.04 g) in 85% yield.

後処理

  1. customThe reaction mixture was quenched with saturated NH4Cl and solvent
  2. concentrationwas concentrated under reduced pressure
  3. extractionAqueous layer was extracted with ethyl acetate and organic layer
  4. washwas washed with brine
  5. dry with materialdried over Na2SO4
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by preparative HPLC

出典と根拠

ORDレコード
ord-82ba9d2b71b6439eb8dafef31dc2a779
出典データセット
uspto-grants-2014_08
特許番号
US08796290B2

反応ノート

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