참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Urea | HCID 1176 | — |
| 반응물 | Ethyl 2-chloroacetoacetate | HCID 11858 | — |
| 용매 | Methanol | HCID 887 | — |
| 생성물 | Ethyl 2-amino-4-methyl-1,3-oxazole-5-carboxylate | HCID 12753431 | — |
반응 단계
Ethyl 2-chloroacetoacetate (8.0 mL, 59 mmol) was added to a mixture of urea (10.6 g, 176 mmol) in MeOH (40 mL), and the reaction mixture was heated to 66° C. overnight. Upon cooling to room temperature, the solids were collected by filtration and suspended in 1 N aqueous NaOH (50 mL). This was extracted with EtOAc (100 mL). The aqueous layer was brought to pH ˜11 with NaOH and was extracted with EtOAc (3×100 mL). The EtOAc extracts were combined, dried over Na2SO4, filtered, and concentrated under reduced pressure. This gave 5.02 g (50%) of the title compound as a white solid. LC-MS: RT=5.1 min, [M+H]+=171.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08822472B2 |
|---|
| 출처 데이터셋 | uspto-grants-2014_09 |
|---|
| ORD ID | ord-8793415874c847e39dc0ac24a4afed71 |
|---|
| 출처 메모 | uspto-grants-2014_09 |
|---|