참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Potassium Carbonate | HCID 11430 | — |
| 반응물 | 2-(Chloroethoxy)ethanol | HCID 12361 | — |
| 반응물 | tert-Butyl hydroxy(methyl)carbamate | HCID 272414 | — |
| 촉매 | Lithium Bromide | HCID 82050 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 생성물 | HCID 86628343 | HCID 86628343 | 72% |
반응 단계
A mixture of N-Boc-N-methyl hydroxylamine (132 mg, 0.898 mmol), 2-(2-chloroethoxy) ethanol (168 mg, 1.35 mmol), K2CO3 (372 mg, 2.69 mmol) and LiBr (2 mg, 0.018 mmol) in DMF (3 mL) was heated at 100° C. and stirred for 16 h. The resulting mixture was cooled down to room temperature and filtered. The filtrate was concentrated and the residue was purified by silica gel flash column chromatography using 50% EtOAc/hexanes as eluent to afford the desired product as colorless oil (152 mg, 0.647 mmol, 72%). 1H NMR (CDCl3, 400 MHz): 8 (ppm) 1.45 (s, 9H), 2.68 (br s, 1H), 3.08 (s, 3H), 3.57-3.60 (m, 2H), 3.66-3.72 (m, 4H), 3.96-3.99 (m, 2H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US09090643B2 |
|---|
| 출처 데이터셋 | uspto-grants-2015_07 |
|---|
| ORD ID | ord-3f788fc15143441998ede3ffedf8488f |
|---|
| 출처 메모 | uspto-grants-2015_07 |
|---|
