反応式
[CH3:1][O:2][C:3]1[CH:46]=[CH:45][C:6]([C:7]([O:22][CH2:23][C@@H:24]([OH:44])[C@@H:25]([OH:43])[C@@H:26]([O:39][CH2:40][CH2:41][F:42])[C@H:27]([N:30]2[CH:38]=[C:36]([CH3:37])[C:34](=[O:35])[NH:33][C:31]2=[O:32])[CH2:28][OH:29])([C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=2)[C:8]2[CH:13]=[CH:12][C:11]([O:14][CH3:15])=[CH:10][CH:9]=2)=[CH:5][CH:4]=1.N1C=CN=C1.O=P12OP3(OP(OP(O3)(O1)=O)(=O)O2)=O.Cl[Si:67]([CH2:72][CH3:73])([CH2:70][CH3:71])[CH2:68][CH3:69]>CN(C=O)C.CCOC(C)=O>[CH3:15][O:14][C:11]1[CH:12]=[CH:13][C:8]([C:7]([O:22][CH2:23][C@@H:24]([OH:44])[C@@H:25]([O:43][Si:67]([CH2:72][CH3:73])([CH2:70][CH3:71])[CH2:68][CH3:69])[C@@H:26]([O:39][CH2:40][CH2:41][F:42])[C@H:27]([N:30]2[CH:38]=[C:36]([CH3:37])[C:34](=[O:35])[NH:33][C:31]2=[O:32])[CH2:28][OH:29])([C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=2)[C:6]2[CH:45]=[CH:46][C:3]([O:2][CH3:1])=[CH:4][CH:5]=2)=[CH:9][CH:10]=1参加物
7
反応物 4
生成物 1
試薬・触媒・溶媒 2
実験手順
Compound 6, prepared as per the procedures illustrated in Example 13 (2.50 g, 4.00 mmol) was mixed with imidazole (1.36 g, 20.0 mmol) over P2O5 under reduced pressure. This mixture was dissolved in anhydrous DMF (13 mL) and chloro triethylsilane (1.71 mL, 10 mmol) was added. The mixture was stirred at room temperature for 12 hours. The reaction mixture was diluted in EtOAc (100 mL), washed with sat. NaHCO3 (100 mL) and brine (50 mL) then dried over anhydrous Na2SO4, filtered and evaporated. The residue was purified by silica gel column chromatography (50% EtOAc in hexanes) to yield Compound 8 (2.45 g, 82.5%) as a white foam. MS (ES): m/z 760.2 [M+Na]+.
後処理
- washwashed with sat. NaHCO3 (100 mL) and brine (50 mL)
- dry with materialthen dried over anhydrous Na2SO4
- filtrationfiltered
- customevaporated
- customThe residue was purified by silica gel column chromatography (50% EtOAc in hexanes)
出典と根拠
- ORDレコード
- ord-f76691064f6648a099b401fbe0225912
- 出典データセット
- uspto-grants-2013_09
- 特許番号
- US08536320B2
関連ノート
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