Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
3-Bromo-2-methyl-1-propene → N-(tert-butoxycarbonyl)-N-(2-methylprop-2-enyl)glycine tert-butyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 3-Bromo-2-methyl-1-propene | HCID 357785 | — |
| 반응물 | Sodium bis(trimethylsilyl)amide | HCID 2724254 | — |
| 반응물 | tert-Butyl ((tert-butoxycarbonyl)amino)acetate | HCID 4097102 | — |
| 용매 | Dimethylformamide | HCID 6228 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 생성물 | N-(tert-butoxycarbonyl)-N-(2-methylprop-2-enyl)glycine tert-butyl ester | HCID 18316043 | 82.1% |
반응 단계
To a solution of N-(tert-butoxycarbonyl)glycine tert-butyl ester (3.97 g, 17.2 mmol) in DMF (70 mL) at 0° C. was added sodium hexamethyldisilazide (3.78 g, 20.6 mmol) and the resulting mixture was stirred for 25 min., then allowed to warm to room temp. The resulting solution was treated with 3-bromo-2-methylpropene (2.60 mL, 25.7 mmol), stirred at room temp. for 10 min., and diluted with EtOAc (300 mL). The EtOAc solution was sequentially washed with water (4×500 mL) and a saturated NaCl solution (4×500 mL), dried (MgSO4), and concentrated under reduced pressure to afford N-(tert-butoxycarbonyl)-N-(2-methylprop-2-enyl)glycine tert-butyl ester (4.03 g, 82%): TLC (10% EtOAc/hex) Rf0.51.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06353006B1 |
| 출처 데이터셋 | uspto-grants-2002_03 |
| ORD ID | ord-e09cb2a2c9324b9389781078417047af |
| 출처 메모 | uspto-grants-2002_03 |