HCID 67192531、化合物 → HCID 67192793、化合物

HRID 2401310ノート

反応式

HRID 2401310 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].[CH3:29][Mg]Br>C1COCC1>[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]([C:1]([OH:3])([CH3:29])[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 67192531HCID 67192531、化合物HCID 178418573HCID 178418573、化合物2 回

生成物 1

HCID 67192793HCID 67192793、化合物収率 32.4%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

2-(3-Acetyl-phenoxy)-8-cyclopentyl-1-propyl-1,7-dihydro-purin-6-one (0.08 g, 0.21 mmol), was taken in THF. To this was added methyl magnesium bromide (30 μl, 0.25 mmol) drop wise at −70° C. and stirred for 2 hours. Another lot of methyl magnesium bromide (30 μl, 0.25 mmol) was added and stirred further for 2 hours. Reaction was quenched with saturated NH4Cl solution and concentrated to evaporate THF and residue was dissolved in ethyl acetate, washed with water followed by brine and dried over anhydrous Na2SO4. The crude product was purified by preparative TLC to give the product (0.027 g) as an off white solid in 32% yield.

後処理

  1. stirringstirred further for 2 hours
  2. customReaction
  3. customwas quenched with saturated NH4Cl solution
  4. concentrationconcentrated
  5. customto evaporate THF and residue
  6. dissolutionwas dissolved in ethyl acetate
  7. washwashed with water
  8. dry with materialdried over anhydrous Na2SO4
  9. customThe crude product was purified by preparative TLC

出典と根拠

ORDレコード
ord-8c5e3572aedb4ba8bd38c0932dc01850
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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