Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
HRID 324427생성일: 2026년 10월 25일
5-Bromo-2,4-bis(1,1-dimethylethoxy)pyrimidine → (+/-)-5-(9,10-Dihydro-4-hydroxy-2,7-dimethyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-yl)-2,4(1H,3H)-pyrimidinedione
https://huagongshe.com/reaction/324427
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 5-Bromo-2,4-bis(1,1-dimethylethoxy)pyrimidine | HCID 818851 | — |
| 반응물 | 9,10-Dihydro-2,7-dimethyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-one | HCID 22003633 | — |
| 반응물 | Butyllithium | HCID 178418339 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | (+/-)-5-(9,10-Dihydro-4-hydroxy-2,7-dimethyl-4H-benzo[5,6]cyclohepta[1,2-d]oxazol-4-yl)-2,4(1H,3H)-pyrimidinedione | HCID 70113848 | — |
반응 단계
To a solution of the product from example 1 step (vi) (9 g) in dry tetrahydrafuran (100 ml) under nitrogen at −78° C. was added n-butyllithium (2.5M, 14.3 ml) dropwise over 1 min. After 30 min a warm solution of the product from step (v) (6.73 g) in tetrahydrofuran (350 ml) was added rapidly via cannula. After further stirring for 1 h the cooling bath was removed and the mixture allowed to stir at room temperature for 30 min. The reaction mixture was quenched with saturated brine and extracted with ethyl acetate (×2). The combined organic extracts were dried over magnesium sulphate and solvent removed under reduced pressure to leave a pale yellow foam. This was dissolved in acetic acid (100 ml) and stired at room temperature for 16 h. The solvent was evaporated under reduced pressure and the residue azeotroped with toluene (×2) to remove last traces of acetic acid. The remaining residue was triturated with diethyl ether/isohexane mixtures and filtered to give the subtitle product as a beige solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06218376B1 |
|---|
| 출처 데이터셋 | uspto-grants-2001_04 |
|---|
| ORD ID | ord-65e682c4b4124404abedce50eb29b36c |
|---|
| 출처 메모 | uspto-grants-2001_04 |
|---|