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HRID 218486作成日:2026年10月25日

Aluminium lithium hydride → HCID 178428426、化合物

https://huagongshe.com/reaction/218486

反応式

関与物質

役割名称HCID仕込み量
反応物Aluminium lithium hydrideHCID 21226445—
反応物5-(3,5-dicyano-1,4-dihydro-2,6-dimethyl-4-pyridinyl)-N-methoxy-N-methyl-1H-indazole-3-carboxamideHCID 24961663—
溶媒TetrahydrofuranHCID 8028—
生成物HCID 178428426HCID 17842842670.1%

反応条件

温度60 °C

反応手順

Lithium aluminum hydride (45 mg, 1.2 mmol) was added portion-wise to a cooled solution of 5-(3,5-dicyano-1,4-dihydro-2,6-dimethyl-4-pyridinyl)-N-methoxy-N-methyl-1H-indazole-3-carboxamide (340 mg, 0.94 mmol) in THF (20 mL). After 30 min, the mixture was heated up to 60° C. After 2 hr, the reaction was quenched by the slow addition of ethyl acetate at 5° C. and 0.4 N NaHSO4. The organic layer was washed with brine, dried with Na2SO4, and concentrated. The crude product was purified by column to give 4-(3-formyl-1H-indazol-5-yl)-1,4-dihydro-2,6-dimethyl-3,5-pyridinedicarbonitrile (200 mg, 70%) (Cpd. No. 145, Table 2). 1H-NMR (400 MHz, DMSO-D6): δ=10.18 (s, 1H), 9.58 (s, 1H), 7.98 (d, 1H), 7.76 (d, 1H), 7.46 (d, 1H), 4.65 (s, 1H), 2.03 (s, 6H) ppm.

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US08198456B2
出典データセットuspto-grants-2012_06
ORD IDord-25fdf6d176984ac792c03a714fd7e2b1
出典メモuspto-grants-2012_06