Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 3-(6-Chloro-pyrazin-2-yloxymethyl)-benzonitrile
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Sodium hydride | HCID 24758 | — |
| 반응물 | 2,6-Dichloropyrazine | HCID 78504 | — |
| 반응물 | 3-(Hydroxymethyl)benzonitrile | HCID 2734677 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 3-(6-Chloro-pyrazin-2-yloxymethyl)-benzonitrile | HCID 22481973 | — |
반응 단계
To a solution of 3-hydroxymethyl-benzonitrile (2.0 g, 15.0 mmol) and 2,6-dichloro-pyrazine (2.24 g, 15.0 mmol) in THF (150 mL) was added 60% NaH in mineral oil (0.9 g, 22.5 mmol). After stirring at ambient temperature for 2 h, the reaction mixture was poured into 1N HCl (100 mL) and extracted with Ethyl Acetate (1×250 mL). The organic layer was washed with brine, dried (Na2SO4), filtered, and concentrated to dryness. The crude material was chromatographed over Silica Gel (40 g) eluting with hexanes (1000 mL) followed by ethyl acetate (500 mL) to obtain 3.53 g of the desired pure product (I-3a) as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06894050B2 |
| 출처 데이터셋 | uspto-grants-2005_05 |
| ORD ID | ord-ecd8b6d06012422eaeba14a71b48fdf5 |
| 출처 메모 | uspto-grants-2005_05 |