반응식
[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]=1참가 물질
5
반응물 3
생성물 1
시약·촉매·용매 1
실험 절차
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.
후처리
- customthe solvent was removed in vacuo
- washwashed with water (3×5 mL)
- dry with materialThe ethyl acetate layer was dried
- filtrationfiltered
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-0ef70621c5d8428ba9a0501e688a9681
- 출처 데이터셋
- uspto-grants-2009_08
- 특허 번호
- US07569578B2
연결된 노트
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