참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Hydroxide | HCID 14797 | — |
| 반응물 | Stannous chloride dihydrate | HCID 61436 | — |
| 반응물 | 6-Methoxy-3-pyridinylamine | HCID 81121 | — |
| 반응물 | Sodium Nitrite | HCID 23668193 | — |
| 용매 | Hydrochloric Acid | HCID 313 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 5-Hydrazinyl-2-methoxypyridine | HCID 22217853 | 91.6% |
반응 단계
5-Amino-2-methoxypyridine (5.0 g, 40 mmol) was dissolved in 6 N HCl (10 mL), cooled to 0° C., and vigorously stirred throughout the procedure. Sodium nitrite (2.8 g, 41 mmol) was dissolved in water (10 mL) and this solution was added to the reaction solution. After 30 min, tin (II) chloride dihydrate (52 g, 230 mmol) in 6 N HCl (20 mL) was added, and the reaction slurry was stirred at 0° C. for 2.5 h. The pH was adjusted to 13 with 40% aqueous potassium hydroxide solution. Ethyl ether was added and the mixture was extracted with EtOAc (4×70 mL), dried (MgSO4) and concentrated to give 5-hydrazino-2-methoxypyridine as an orange solid (5.1 g).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06656933B2 |
|---|
| 출처 데이터셋 | uspto-grants-2003_12 |
|---|
| ORD ID | ord-64e9bbe8871d426f8a4e0cc02f8f16bb |
|---|
| 출처 메모 | uspto-grants-2003_12 |
|---|
