Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Methyl 4-[amino(hydroxyimino)methyl]-2-fluorobenzoate → tert-butyl N-[[3-[(Z)-N'-hydroxycarbamimidoyl]phenyl]methyl]-N-(2-hydroxyethyl)carbamate
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Methyl 4-[amino(hydroxyimino)methyl]-2-fluorobenzoate | HCID 76644654 | — |
| 반응물 | tert-Butyl 3-cyanobenzyl(2-hydroxyethyl)carbamate | HCID 86645651 | — |
| 생성물 | tert-butyl N-[[3-[(Z)-N'-hydroxycarbamimidoyl]phenyl]methyl]-N-(2-hydroxyethyl)carbamate | HCID 59495768 | — |
반응 단계
Title compound was prepared following procedure described for Intermediate 1 step 2 but starting from tert-Butyl 3-cyanobenzyl(2-hydroxyethyl)carbamate obtained from step 2 (6 g, 0.0217 mol) (RT for 12 h). Reaction mixture was concentrated under reduced pressure and purified by column chromatography using silica gel and chloroform/methanol as a eluent to afford the title compound as a white solid. 1H NMR (DMSO-d6, 400 MHz) δ 9.60 (s, 1H), 7.52-7.53 (m, 2H), 7.31-7.34 (m, 1H), 7.19-7.20 (m, 1H), 5.76 (s, 1H), 4.65-4.68 (m, 1H), 4.42 (s, 2H), 3.42-3.47 (m, 2H), 3.13-3.16 (m, 2H), 1.33-1.41 (m, 9H). LC/MS (Method A): 310.0 (M+H)+. HPLC (Method B) Rt 4.57 min (Purity: 94.1%).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08202865B2 |
| 출처 데이터셋 | uspto-grants-2012_06 |
| ORD ID | ord-99d4c005d5bc4da3bf2fb0251a64783e |
| 출처 메모 | uspto-grants-2012_06 |