참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrogen Bromide | HCID 260 | — |
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | 2-Bromo-1,1-dimethoxyethane | HCID 81672 | — |
| 반응물 | 2-Amino-6-Chloropyrazine | HCID 118458 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 촉매 | Water | HCID 962 | — |
| 용매 | Isopropanol | HCID 3776 | — |
| 용매 | Hexane | HCID 8058 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | 5-Chloroimidazo[1,2-A]pyrazine | HCID 12841588 | 25.31% |
반응 단계
NaHCO3 (4.215 g, 50.1736 mmol) and IPA (40 mL) were added to a mixture of 2-bromo-1,1-dimethoxy-ethane (6.37 mL, 10.8066 mmol), 40% HBr (475 mL, 2.3157 mmol) and 2 drops of water previously refluxed for 1 hr. The reaction mixture was stirred for 5 mins and filtered. To the filtrate was added 6-chloro-pyrazin-2-ylamine (1 g, 7.7190 mmol) and the resulting mixture was refluxed for overnight. The reaction was monitored by TLC (50% ethylacetate in hexane). The reaction mixture was neutralized with Na2CO3 and partitioned between ethylacetate and water. The organic layer was washed with water, brine, dried over Na2SO4 and concentrated. Purification by column chromatography on silica gel (1-2% MeOH in CHCl3) afforded 300 mg of the product (25.31% yield).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | USRE045173E1 |
|---|
| 출처 데이터셋 | uspto-grants-2014_09 |
|---|
| ORD ID | ord-fe65c3a1d8c0408b94f2bf59208ad84f |
|---|
| 출처 메모 | uspto-grants-2014_09 |
|---|
