Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triethylamine → 6-(Hydroxymethyl)-2H-pyrido[3,2-b][1,4]thiazin-3(4H)-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triethylamine | HCID 8471 | — |
| 반응물 | Isobutyl chloroformate | HCID 62365 | — |
| 반응물 | 3-Oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]thiazine-6-carboxylic acid | HCID 21873787 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 6-(Hydroxymethyl)-2H-pyrido[3,2-b][1,4]thiazin-3(4H)-one | HCID 11608093 | 74.1% |
반응 단계
A solution of 3-Oxo-3,4-dihydro-2H-pyrido[3,2-b][1,4]thiazine-6-carboxylic acid (500 mg) in THF (24 mL) with triethylamine (0.396 mL) was cooled to −10° C. and isobutyl chloroformate (0.339 ml) added. After 20 minutes the suspension was filtered through kieselguhr into an ice-cooled solution of sodium borohydride (272 mg) in water (8 mL), the mixture stirred 30 minutes and the pH reduced to 7 with dilute HCl. The solvent was evaporated and the residue triturated under water. The product was filtered and dried under vacuum to give a white solid (346 mg); MS (APCl−) m/z 195 ([M−H]−, 50%), 165(100%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07691850B2 |
| 출처 데이터셋 | uspto-grants-2010_04 |
| ORD ID | ord-2c0a4184e7ae4663ae54c2acb62497bb |
| 출처 메모 | uspto-grants-2010_04 |