Iodine → HCID 178497289、化合物
反応式
[NH:1]1[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([C:10]([O:12][CH3:13])=[O:11])[CH:8]=2)[CH:3]=[N:2]1.[I:14]I.[OH-].[K+]>CC(N(C)C)=O>[I:14][C:3]1[C:4]2[C:9](=[CH:8][C:7]([C:10]([O:12][CH3:13])=[O:11])=[CH:6][CH:5]=2)[NH:1][N:2]=1参加物
5
実験手順
To a solution of methyl 1H-indazole-6-carboxylate D-2 (5.0 g, 28 mmol) in DMAC (50 mL) at 0° C. was added iodine (14.4 g, 56.7 mmol) and potassium hydroxide (6.3 g, 114 mmol) portionwise. After addition, the mixture was kept stirring for 1 h, then quenched with aq. Na2S2O3 and extracted with EtOAc. The combined organics were concentrated and trituated with hexane. The precipitate was collected by filtration to afford the title compound as a brown solid. LCMS (ESI) calc'd for C9H8IN2O2 [M+H]+: 302.9. found: 302.9.
後処理
- additionAfter addition
- customquenched with aq. Na2S2O3
- extractionextracted with EtOAc
- concentrationThe combined organics were concentrated
- filtrationThe precipitate was collected by filtration
出典と根拠
- ORDレコード
- ord-00e3a1924ef04cab9085661c7d2f8352
- 出典データセット
- uspto-grants-2015_08
- 特許番号
- US09095583B2
反応ノート
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