Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methoxydiphenylphosphine → 5-Bromo-4-diphenylphosphinyl-2-methylthiopyrimidine
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methoxydiphenylphosphine | HCID 77636 | — |
| 반응물 | 5-Bromo-4-chloro-2-(methylsulfanyl)pyrimidine | HCID 265881 | — |
| 용매 | 1,2-Dichlorobenzene | HCID 7239 | — |
| 생성물 | 5-Bromo-4-diphenylphosphinyl-2-methylthiopyrimidine | HCID 20539470 | 49.3% |
반응 단계
To a stirred, refluxing mixture of 3.56 g of 5-bromo-4-chloro-2-methylthiopyrimidine in 100 ml of o-dichlorobenzene under nitrogen was added dropwise 10.00 g of methyl diphenylphosphinite. After the addition was completed, the mixture was refluxed for 6 hours and then allowed to cool. Volatiles were removed from the mixture under vacuum, and the residue was recrystallized from 30 ml of 1-chlorobutane and dried at 50° C./0.1 mm (13 Pa) to give 2.97 g of 5-bromo-4-diphenylphosphinyl-2-methylthiopyrimidine (shown by formula in Claim 7) as white crystals, mp 124°-127° C. Anal. Calcd for C17H14BrN2OPS: C, 50.39; H, 3.48; N, 6.91. Found: C, 50.54; H, 3.67; N, 6.84.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US04234729 |
| 출처 데이터셋 | uspto-grants-1980_11 |
| ORD ID | ord-b1dcd8c8a1f44f40af31fe94fd18ce6a |
| 출처 메모 | uspto-grants-1980_11 |