참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Thionyl Chloride | HCID 24386 | — |
| 반응물 | Sodium Sulfate | HCID 24436 | — |
| 반응물 | (3,5-Dimethyl-4-nitropyridin-2-yl)methanol | HCID 4049415 | — |
| 용매 | Acetonitrile | HCID 6342 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 2-(Chloromethyl)-3,5-dimethyl-4-nitropyridine | HCID 11217896 | — |
반응 단계
8.0 ml (0.11 mole) of thionyl chloride in 20.0 ml of methylenechloride was added to a solution of 20.0 gms 2-hydroxymethyl-3,5dimethyl-4-nitropyridine, of formula-II obtained in step-(a), at temperature of 10-15° C. over a period of 1 hr. The reaction is maintained at 10-15° C. for further 30 min. Aqueous 10% solution of sodium carbonate was slowly added to the reaction mixture at 10-15° C. and pH adjusted to 8.0 to 8.5. The organic base (compound) is over anhydrous sodium sulfate and solvent was removed under vacuum to obtain crude product. (purity 85%) Pure compound is isolated by re-crystallization from acetonitrile.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06303787B1 |
|---|
| 출처 데이터셋 | uspto-grants-2001_10 |
|---|
| ORD ID | ord-dcdd1b239c514d568bf8d119fa91e1f4 |
|---|
| 출처 메모 | uspto-grants-2001_10 |
|---|
