참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 1-(2-Bromoethyl)-3-chlorobenzene | HCID 140140 | — |
| 반응물 | (S)-8-(Morpholin-4-yl)-2-(trifluoromethyl)-1,2,3,4-tetrahydropyrimido[1,2-a]pyrimidin-6-one | HCID 136238743 | — |
| 촉매 | Tetrabutylammonium hydrogen sulfate | HCID 94433 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | HCID 49854610 | HCID 49854610 | 19.2% |
반응 단계
The product is prepared according to the procedure described in Example 40, using 150 mg of (8S)-2-(morpholin-4-yl)-8-(trifluoromethyl)-6,7,8,9-tetrahydro-4 H-pyrimido[1,2-a]pyrimidin-4-one in 2.5 ml of toluene are added 296 mg of sodium hydroxide in 2.5 ml of water, 33 mg of tetrabutylammonium hydrogen sulphate and 216 mg of 1-(2-bromoethyl)-3-chlorobenzene. After 44 hours at 60° C. After cooling, the reaction mixture is diluted with ethyl acetate. The organic phase is separated and the aqueous phase is extracted with ethyl acetate. The combined organic phases are concentrated to dryness under reduced pressure and the residue is purified by preparative HPLC/MS (Method D). 42 mg of (8S)-9-[2-(3-chloro-phenyl)ethyl]-2-(morpholin-4-yl)-8-(trifluoromethyl)-6,7,8,9-tetrahydro-4 H-pyrimido[1,2-a]pyrimidin-4-one are thus obtained, the characteristics of which are the following:
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08846670B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_09 |
|---|
| ORD ID | ord-324f1ced10c6442d886e75302abf13e7 |
|---|
| 출처 메모 | uspto-grants-2014_09 |
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