反応式
[CH3:1][N:2]([CH3:32])[C:3]([CH3:31])([CH2:22][O:23][Si](C(C)(C)C)(C)C)[CH:4]([NH:11][C:12](=[O:21])[C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([CH3:19])[C:14]=1[CH3:20])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1.[F-].C([N+](CCCC)(CCCC)CCCC)CCC.C(OCC)(=O)C.CCCCC>C1COCC1>[CH3:32][N:2]([CH3:1])[C:3]([CH3:31])([CH2:22][OH:23])[CH:4]([NH:11][C:12](=[O:21])[C:13]1[CH:18]=[CH:17][CH:16]=[C:15]([CH3:19])[C:14]=1[CH3:20])[C:5]1[CH:6]=[CH:7][CH:8]=[CH:9][CH:10]=1参加物
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
A solution of (±)-N-(2-(dimethylamino)-3-{[(1,1-dimethylethyl)(dimethyl)silyl]oxy}-2-methyl-1-phenylpropyl)-2,3-dimethylbenzamide D49 (56 mg; 0.12 mmol) in THF (5 ml) was treated with a solution of tetrabutylammonium fluoride (1.0M solution in THF; 0.2 ml, 0.2 mmol) and the mixture stirred at room temperature overnight. The mixture was poured directly onto a chromatography column (Flashmaster II; eluent 0-100% ethyl acetate/pentane) to afford the title compound (38 mg; 63%). 1H NMR (CDCl3) δ: 0.73 and 1.14 (3H, 2×s), 1.70-2.50 (1H, br s), 2.26 (6H, q), 2.38 and 2.48 (6H, 2×s), 3.17, 3.39, and 3.55 (2H, 3×d), 5.26 and 5.46 (1H, 2×d), 6.83 and 7.89 (1H, 2×br d), 7.07-7.46 (8H, br m). Mass spectrum (Electrospray LC/MS), API+: Found 341 (MH+), C21H28N2O2Si requires 340. Ret. time 1.71 and 1.76 min.
出典と根拠
- ORDレコード
- ord-814de7e612604058bc344bbc4f28f597
- 出典データセット
- uspto-grants-2010_06
- 特許番号
- US07745642B2
関連ノート
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