Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
1,2-Dichloroethane → Boc-D-Ala-NH2
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 1,2-Dichloroethane | HCID 11 | — |
| 반응물 | Ammonia | HCID 222 | — |
| 반응물 | 4-Methylmorpholine | HCID 7972 | — |
| 반응물 | 1,4-Dioxane | HCID 31275 | — |
| 반응물 | 1-Hydroxybenzotriazole | HCID 75771 | — |
| 반응물 | BOC-D-alanine | HCID 637606 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | Boc-D-Ala-NH2 | HCID 7015296 | 23.02% |
반응 단계
(R)-2-(tert-Butoxycarbonylamino)propanoic acid (1 g, 5.29 mmol), EDC (1.216 g, 6.34 mmol), and HOBt (0.971 g, 6.34 mmol) were dissolved in CH2Cl2 (5 mL). Ammonia (0.5 M) in dioxane (52.9 mL, 26.4 mmol) and 4-methylmorpholine (3.49 mL, 31.7 mmol) were added to the reaction mixture. After stirring for 1 h, the solvent was removed and ethyl acetate was added. This was washed with brine and saturated NaHCO3 solution. The organic layer was dried and concentrated to provide the product (R)-tert-butyl 1-amino-1-oxopropan-2-ylcarbamate (Int-X-A, 229 mg, 1.217 mmol, 23.02% yield); [M+Na]+=211.2; 1H NMR (400 MHz, methanol-d4) δ ppm 4.06 (1 H, q), 1.44 (9 H, s), 1.31 (3 H, d, J=7.04 Hz).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08835470B2 |
| 출처 데이터셋 | uspto-grants-2014_09 |
| ORD ID | ord-09a01529d70343c09047cf86e627c1cc |
| 출처 메모 | uspto-grants-2014_09 |