Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Dimethyl Sulfoxide → 1-Cyclopentyl-7-(4-methoxyphenylamino)-3,4-dihydro-pyrimido[4,5-d]pyrimidin-2(1H)-one
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Dimethyl Sulfoxide | HCID 679 | — |
| 반응물 | P-Anisidine | HCID 7732 | — |
| 반응물 | 1-cyclopentyl-7-methanesulfinyl-3,4-dihydro-pyrimido[4,5-d]pyrimidin-2(1H)-one | HCID 68859342 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 1-Cyclopentyl-7-(4-methoxyphenylamino)-3,4-dihydro-pyrimido[4,5-d]pyrimidin-2(1H)-one | HCID 53635730 | 24.2% |
반응 단계
A solution of 300 mg (1.07 mmol) of 1-cyclopentyl-7-methanesulfinyl-3,4-dihydro-pyrimido[4,5-d]pyrimidin-2(1H)-one, 527 mg (4.28 mmol) of p-anisidine, and 1.5 mL of dimethyl sulfoxide is heated at 130° C. for 30 hours, then cooled and diluted with ethyl acetate. The mixture is washed three times with aqueous sodium chloride solution, dried over magnesium sulfate, and concentrated. The residual solids are washed with 9:1:0.1:0.1 chloroform/ethyl acetate/ethanol/triethylamine then with chloroform, and suspended in 150 mL of 7:3 chloroform/methanol. The suspension is diluted with 20 mL of hexane, stirred for 3 hours, and filtered to afford 88 mg (24%) of the title compound as an off-white powder: mp 247-249° C. (dec).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07501425B1 |
| 출처 데이터셋 | uspto-grants-2009_03 |
| ORD ID | ord-e24d2764068143ee8d95a30d04645eb4 |
| 출처 메모 | uspto-grants-2009_03 |