Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Triphenylphosphine dibromide → 5-Bromo-3-(5-phenyl-1,3,4-thiadiazol-2-yl)pyrazin-2-amine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Triphenylphosphine dibromide | HCID 70579 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | N-aminobenzenecarbothioamide | HCID 3361911 | — |
| 반응물 | 3-Amino-6-bromopyrazine-2-carboxylic acid | HCID 18521600 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 생성물 | 5-Bromo-3-(5-phenyl-1,3,4-thiadiazol-2-yl)pyrazin-2-amine | HCID 59471891 | 43% |
반응 단계
3-amino-6-bromo-pyrazine-2-carboxylic acid (1.000 g, 4.588 mmol) and benzenecarbothiohydrazide (759.1 mg, 4.588 mmol) were suspended in acetonitrile (25.00 mL), cooled in an ice bath and then treated with dibromo-triphenyl-phosphorane (4.453 g, 10.55 mmol) The reaction mixture was allowed to stir in an ice bath for 2 hours and then DIPEA (1.778 g, 2.396 mL, 13.76 mmol) was added slowly at 10° C. The reaction was left to stir at 0-10° C. for a further hour and the resultant precipitate was isolated by filtration, washed with a small amount of acetonitrile and dried (659 mg, 43% Yield). MS (ES+) 335.93
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08841308B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-87db2c5641a543e298f4bac069230a5a |
| 출처 메모 | uspto-grants-2014_09 |