反応式
[Cl:1][C:2]1[N:10](CC=C)[C:9]2[C:8](=[O:14])[NH:7][C:6](=[O:15])[N:5]([CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])[C:4]=2[N:3]=1.[Cl:21][C:22]1[CH:27]=[CH:26][C:25]([CH2:28][C:29]2[N:33]=[C:32]([CH2:34][CH2:35][CH2:36]O)[O:31][N:30]=2)=[CH:24][CH:23]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH:57]1[CH:62]=[CH:61][C:60]([CH2:63][O:64][C:65](/[N:67]=[N:68]/[C:69]([O:71][CH2:72][C:73]2[CH:78]=[CH:77][CH:76]=[CH:75][CH:74]=2)=[O:70])=[O:66])=[CH:59][CH:58]=1>C1COCC1>[Cl:1][C:2]1[NH:10][C:9]2[C:8](=[O:14])[N:7]([CH2:36][CH2:35][CH2:34][C:32]3[O:31][N:30]=[C:29]([CH2:28][C:25]4[CH:24]=[CH:23][C:22]([Cl:21])=[CH:27][CH:26]=4)[N:33]=3)[C:6](=[O:15])[N:5]([CH2:16][CH2:17][CH2:18][CH2:19][CH3:20])[C:4]=2[N:3]=1.[CH:76]1[CH:75]=[CH:74][C:73]([CH2:72][O:71][C:69](/[N:68]=[N:67]/[C:65]([O:64][CH2:63][C:60]2[CH:61]=[CH:62][CH:57]=[CH:58][CH:59]=2)=[O:66])=[O:70])=[CH:78][CH:77]=1参加物
7
反応物 4
生成物 2
試薬・触媒・溶媒 1
実験手順
To a solution of 8-chloro-3-pentyl-7-(2-propen-1-yl)-3,7-dihydro-1H-purine-2,6-dione (0.10 g, 0.34 mmol), 3-{3-[(4-chlorophenyl)methyl]-1,2,4-oxadiazol-5-yl}-1-propanol (0.086 g, 0.34 mmol) and triphenylphosphine (0.186 g, 0.69 mmol) in THF (5 ml) was added dibenzylazodicarboxylate (0.204 g, 0.68 mmol) and the solution stirred for 18 h. The solution was then concentrated and the residues chromatographed over silica (20 g, SPE) eluting with DCM initially then DCM/Et2O mixtures to yield the title compound contaminated with dibenzylazodicarboxylate by-products (0.18 g). Material used crude in deprotection step.
後処理
- concentrationThe solution was then concentrated
- customthe residues chromatographed over silica (20 g, SPE)
- washeluting with DCM initially
出典と根拠
- ORDレコード
- ord-981292021ff24f748c5004279100e538
- 出典データセット
- uspto-grants-2012_03
- 特許番号
- US08143264B2
関連ノート
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