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Sodium borohydride → 1-tosyl-4,5,6,7-tetrahydro-1H-indazol-4-ol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium borohydride | HCID 4311764 | — |
| 反応物 | 1-tosyl-6,7-dihydro-1H-indazol-4(5H)-one | HCID 67458588 | — |
| 溶媒 | Tetrahydrofuran ethanol | HCID 21873804 | — |
| 生成物 | 1-tosyl-4,5,6,7-tetrahydro-1H-indazol-4-ol | HCID 90304168 | 98.2% |
反応手順
To a solution of 1-tosyl-6,7-dihydro-1H-indazol-4(5H)-one (5 g, 17.22 mmol) in EtOH/THF (30 mL/30 mL)) was added NaBH4 (1.3 g, 34.44 mmol) under ice-bath. The mixture was stirred for 1 h at this temperature and quenched with aqueous NH4Cl solution. Removed the solvent under reduced pressure and extracted with DCM and the combined organic layer was washed with water, brine and dried over anhydrous Na2SO4. The organic layer was concentrated in vacuo and the residue 1-tosyl-4,5,6,7-tetrahydro-1H-indazol-4-ol (4.94 g, yield 98.2%) was used directly to next step. MS-ESI (m/z): 293 (M+1)+ (Acq Method: 10-80AB_2 min; Rt: 1.01 min)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09446130B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-79a1b44a121d45a4a7859a7efd3e18eb |
| 出典メモ | uspto-grants-2016_09 |