Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Bromine → 4-methoxy-N7-methyl-N7-(tetrahydro-pyran-4-ylmethyl)-benzothiazole-2,7-diamine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Bromine | HCID 24408 | — |
| 반응물 | HCID 22736994 | HCID 22736994 | — |
| 용매 | Chloroform | HCID 6212 | — |
| 생성물 | 4-methoxy-N7-methyl-N7-(tetrahydro-pyran-4-ylmethyl)-benzothiazole-2,7-diamine | HCID 22737005 | 98.2% |
반응 단계
1.5 g (0.53 mmol) {2-methoxy-5-[methyl-(tetrahydro-pyran-4-ylmethyl)-amino]-phenyl}-thiourea were dissolved in 15 ml chloroform and at room temperature 0.025 ml (0.5 mmol) Br2 were added slowly. After 24 hrs of reflux the mixture was concentrated in vactio and the residue suspended in water. Sodium bicarbonate solution was added until the pH was 10, and the crystals were collected by filtration. These were subjected to column chromatography (1/1 hexane/ethyl acetate) to afford 0.16 g (10%) of 4-methoxy-N7-methyl-N7-(tetrahydro-pyran-4-ylmethyl)-benzothiazole-2,7-diamine as brown solid. ES-MS m/e (%): 308 (M+H+, 100).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06713499B2 |
| 출처 데이터셋 | uspto-grants-2004_03 |
| ORD ID | ord-ff07b51b7c5147e79cbabb50bbbdd643 |
| 출처 메모 | uspto-grants-2004_03 |