참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Ethyl 3-aminobenzoate | HCID 11400 | — |
| 반응물 | 6-(2,6-Dichlorophenyl)-8-methyl-2-methylsulfonyl-8H-pyrido[2,3-d]pyrimidin-7-one | HCID 10596157 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 2-aminopyrido[2,3-d]pyrimidin-7(8H)-one 55 | HCID 5327901 | — |
반응 단계
A mixture of 0.226 g (0.58 mmol) of 6-(2,6-dichlorophenyl)-2-methanesulfonyl-8-methyl-8H-pyrido[2,3-d]pyrimidin-7-one of Example 39 and 0.40 g (2.42 mmol) of 3-aminobenzoic acid, ethyl ester was fused in a 170° C. oil bath to give a clear melt. After 6 minutes, the melt was cooled to ca. 100° C. Glacial acetic acid (1 mL) was added to dissolve the melt. Water (5 mL) was added to precipitate a solid. The solid was filtered, washed well with water, and triturated with 2 mL of methanol. The mixture was filtered, and the cake was washed with 1 mL of methanol and then ether; wt 0.194 g. Recrystallization from ethyl acetate gave pure product; wt 0.075 g; mp 238°-240° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US05733914 |
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| 출처 데이터셋 | uspto-grants-1998_03 |
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| ORD ID | ord-9fd5cd2b22e5454fb149f6f3ed738293 |
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| 출처 메모 | uspto-grants-1998_03 |
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