참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Methyl benzo[d]thiazole-6-carboxylate | HCID 595763 | — |
| 반응물 | Aluminium lithium hydride | HCID 21226445 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 6-(Hydroxymethyl)benzothiazole | HCID 17860385 | 99% |
반응 단계
Add slowly a solution of benzothiazole-6-carboxylic acid methyl ester (0.5 g, 2.59 mmol) in anhydrous THF (10 mL) to a suspension of lithium aluminum hydride (0.1 g, 2.85 mmol) in anhydrous THF (20 mL) at −10° C. and stir for 20 min at −10° C. Treat the reaction mixture with 2N aqueous NaOH until a granular precipitate starts to form and filter through a pad of Celite®. Evaporate the solvent and purify by chromatography on silica gel eluting with hexane/EtOAc (1:0, 9:1, 4:1, 7:3, 3:2 and 1:1) to obtain the desired intermediate as a yellow oil (0.4 g, 99%). MS (ES+) m/z: 166 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08022062B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_09 |
|---|
| ORD ID | ord-ddcd779d55db429da89e393769149eb4 |
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| 출처 메모 | uspto-grants-2011_09 |
|---|
