참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 1,1-Dimethylethyl 2-[(4-methoxyphenyl)methyl]hydrazinecarboxylate | HCID 10753314 | — |
| 용매 | 1,4-Dioxane | HCID 31275 | — |
| 생성물 | (4-Methoxybenzyl)hydrazine dihydrochloride | HCID 22747476 | 98% |
반응 단계
To a solution of 4 N hydrogen chloride in dioxane (2000 mL, 8.00 mol HCl), add tert-butyl 2-(4-methoxybenzyl)hydrazinecarboxylate (324 g, 1.09 mol) dissolved in a minimal amount of dioxane, slowly over a period of 1 h. A precipitate gradually forms. Allow the solution to stir 16 h at 20±5° C. Collect the solids by filtration. Slurry the solids in heptane (2000 mL) and isolate the solids by filtration. Dry the solids using a nitrogen press to give the title compound (242.3 g, 1.08 mol, 98%). 1H NMR (400 MHz, DMSO-d6) δ 8.2-9.0 (bs, 5H), 7.3-7.4 (d, 2H), 6.8-7.0 (d, 2H), 4.0 (s, 2H), 3.7 (s, 3H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07897600B2 |
|---|
| 출처 데이터셋 | uspto-grants-2011_03 |
|---|
| ORD ID | ord-f34e2230563a4c58af21ea9555077c17 |
|---|
| 출처 메모 | uspto-grants-2011_03 |
|---|
