Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl iodide → 6-(6-chloropyrimidine-4-carbonyl)-3,4-dimethyl-3H-benzoxazol-2-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl iodide | HCID 6328 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 6-(6-chloropyrimidine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one | HCID 58181206 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | 6-(6-chloropyrimidine-4-carbonyl)-3,4-dimethyl-3H-benzoxazol-2-one | HCID 58181162 | — |
반응 단계
0.35 g (8.0 mmol) sodium hydride (55%, suspension in mineral oil) were added to 2.2 g (7.6 mmol) of 6-(6-chloropyrimidine-4-carbonyl)-4-methyl-3H-benzoxazol-2-one in 10 mL N,N′-dimethylformamide. The reaction mixture was stirred for 30 min at RT. Then 0.95 mL (15.0 mmol) iodomethane were added and the mixture was stirred for 1 h at RT. The reaction mixture was combined with ice water, the aqueous phase was extracted several times with EtOAc. The combined organic phases were dried on sodium sulphate, filtered and concentrated to dryness by rotary evaporation. The residue was triturated with diethyl ether, suction filtered and dried.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08629137B2 |
| 출처 데이터셋 | uspto-grants-2014_01 |
| ORD ID | ord-3356c125830d411c8dd00e039d488881 |
| 출처 메모 | uspto-grants-2014_01 |