反応式
[CH3:1][C:2]1[CH:3]=[C:4]([CH2:11][CH:12]([CH2:17][C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[C:13]([O:15][CH3:16])=[O:14])[CH:5]=[C:6]2[C:10]=1[NH:9][N:8]=[CH:7]2.C1(N(C)C2CCCCC2)CCCCC1.[CH3:39][Si:40]([CH2:43][CH2:44][O:45][CH2:46]Cl)([CH3:42])[CH3:41]>O1CCCC1>[CH3:1][C:2]1[C:10]2[C:6](=[CH:7][N:8]([CH2:46][O:45][CH2:44][CH2:43][Si:40]([CH3:42])([CH3:41])[CH3:39])[N:9]=2)[CH:5]=[C:4]([CH2:11][CH:12]([CH2:17][C:18]([O:20][C:21]([CH3:24])([CH3:23])[CH3:22])=[O:19])[C:13]([O:15][CH3:16])=[O:14])[CH:3]=1参加物
5
反応物 3
生成物 1
試薬・触媒・溶媒 1
実験手順
To a solution of 4-tert-butyl 1-methyl 2-((7-methyl-1H-indazol-5-yl)methyl)succinate (0.6053 g, 1.82 mmol) and N-cyclohexyl-N-methylcyclohexanamine (0.4686 mL, 2.19 mmol) in tetrahydrofuran (10 mL) was added trimethylsilylethoxymethyl chloride (0.3859 mL, 2.19 mmol) at room temperature under nitrogen. The reaction was stirred overnight and the solvent was removed in vacuo. The crude product was taken up in ethyl acetate (10 mL) and washed with water (3×5 mL). The ethyl acetate layer was dried, filtered and concentrated. The final product was obtained by flash chromatography, eluting with 0% to 20% ethyl acetate/hexane. (0.5873 g, 70%) HPLC tR=1.89 min, MS(ESI)[M+H]+=462.94.
後処理
- customthe solvent was removed in vacuo
- washwashed with water (3×5 mL)
- dry with materialThe ethyl acetate layer was dried
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-0ef70621c5d8428ba9a0501e688a9681
- 出典データセット
- uspto-grants-2009_08
- 特許番号
- US07569578B2
関連ノート
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