Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Diisopropylethylamine → [(S)-1-(Methoxy-methyl-carbamoyl)-2-methyl-propyl]carbamic acid benzyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | N-Carbobenzoxy-L-valine | HCID 726987 | — |
| 반응물 | 1,3-Propanediamine, N'-(ethylcarbonimidoyl)-N,N-dimethyl-, monohydrochloride | HCID 2723939 | — |
| 반응물 | Methoxymethanamine hydrochloride | HCID 21959107 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | [(S)-1-(Methoxy-methyl-carbamoyl)-2-methyl-propyl]carbamic acid benzyl ester | HCID 10469699 | 87.4% |
반응 단계
To (S)-2-benzyloxycarbonylamino-3-methyl-butyric acid (7) (50.0 g, 199 mmol), N-methoxymethylamine hydrochloride (38.8 g, 398 mmol) and EDC.HCl (47.7 g, 249 mmol) in DCM (500 mL) was added DIPEA (87 mL, 497 mmol) and the reaction mixture stirred at ambient temperature for 20 h, after which time the reaction mixture was diluted with DCM (200 mL), washed with 1M HCl (aq) (3×200 mL), 1M NaOH (aq) (200 mL), sat. NaHCO3 (aq) (200 mL) and brine (300 mL). The organic layer was dried over MgSO4, filtered and the solvent removed under vacuum to give the desired compound as a colourless oil (51.2 g, 87%); (AnalpH2_MeOH—4 min) Rt 2.76 min; m/z 295 (MH)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08541363B2 |
| 출처 데이터셋 | uspto-grants-2013_09 |
| ORD ID | ord-a3500c0216c449f7981b9331224c5b24 |
| 출처 메모 | uspto-grants-2013_09 |