Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Ethyl bromoacetate → Tert-butyl 2-(2-ethoxy-2-oxoethyl)hydrazine-1-carboxylate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Ethyl bromoacetate | HCID 7748 | — |
| 반응물 | tert-Butyl carbazate | HCID 70091 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | Tert-butyl 2-(2-ethoxy-2-oxoethyl)hydrazine-1-carboxylate | HCID 13434344 | 70% |
반응 단계
Ethyl bromoacetate 3 (6.97 mL, 62.8 mmol) was added to a stirred solution of tert-butylcarbazate 2 (24.9 g, 188.6 mmol) in water (25 mL) at room temperature. The mixture was stirred for 30 min. Water layer was then extracted with ethyl acetate (3×). Ethyl acetate extracts were pooled together and washed with brine. Ethyl acetate was evaporated under vacuum to get crude product which was purified by flash column chromatography using hexane:ethyl acetate (70:30) as an eluent (yield 70%). 1H NMR (500 MHz, CDCl3) 1.28 (3H, CH2—CH3, t), 1.45 (9H, C—CH3, s), 3.64 (2H, NH—CH2—CO, s), 4.20 (2H, CH2CH3, q); MS Anal. Mol. Wt. 218.25 (M+1).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08785499B2 |
| 출처 데이터셋 | uspto-grants-2014_07 |
| ORD ID | ord-632fadc7fdcc47aeb266649656096a00 |
| 출처 메모 | uspto-grants-2014_07 |