Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Potassium Phosphate, Tribasic → 6-(2-Chloro-pyrimidin-4-yloxy)-benzo[d]isoxazole-3-carboxylic acid ethyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Potassium Phosphate, Tribasic | HCID 62657 | — |
| 반응물 | 2,4-Dichloropyrimidine | HCID 77531 | — |
| 반응물 | Ethyl 6-hydroxybenzo[d]isoxazole-3-carboxylate | HCID 136216618 | — |
| 용매 | Citric Acid | HCID 311 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 생성물 | 6-(2-Chloro-pyrimidin-4-yloxy)-benzo[d]isoxazole-3-carboxylic acid ethyl ester | HCID 86626624 | — |
반응 단계
A suspension of 2.7 g (18.1 mMol) 2,4-dichloropyrimidine, 4.12 g (19.9 mMol) 6-hydroxy-benzo[d]isoxazole-3-carboxylic acid ethyl ester [preparation see: J. Am. Chem. Soc. 97 (1974), 7305] and 8.45 g (39.8 mMol) K3PO4 in 90 ml NMP is stirred for 22 h at rt. Then the mixture is diluted with 0.5 l CH2Cl2 and 0.9 l of a 5% citric acid solution. The organic phase is separated off, washed with water and brine, dried (Na2SO4) and concentrated. Column chromatography (SiO2; CH2Cl2) gives the title compound: MS: [M+1]+=320; TLC(CH2Cl2/EtOAc 49:1): Rf=0.42.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08058276B2 |
| 출처 데이터셋 | uspto-grants-2011_11 |
| ORD ID | ord-4963a6315e6c473497aba41396a320b8 |
| 출처 메모 | uspto-grants-2011_11 |