참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Sodium Carbonate | HCID 10340 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | Perchloric Acid | HCID 24247 | — |
| 반응물 | (2S)-2-Amino-4,4-dimethylpentanoic acid | HCID 194032 | — |
| 반응물 | HCID 20476630 | HCID 20476630 | — |
| 용매 | Methanol | HCID 887 | — |
| 용매 | Toluene | HCID 1140 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Ethyl Acetate | HCID 8857 | — |
| 용매 | tert-Butyl acetate | HCID 10908 | — |
| 생성물 | HCID 54211560 | HCID 54211560 | 96% |
반응 단계
4-Methylleucine (500 mg, 3.44 mmol) was suspended in 10 ml t-butyl acetate. Perchloric acid (0.2 ml, 3.49 mmol) was added and the flask was stopped with a septum and stirred over night. Analysis was performed using TLC DCM:MeOH, 9:1; staining with a ninhydrine/EtOH solution). The solution was poured into a flask containing 30 ml EtOAc and 30 ml 5% Na2CO3. The aq-layer turned acidic and 2M NaOH was added until pH was approximately 7. The phases were separated and the aq-phase was washed with 2×30 ml EtOAc. The combined organic phases were washed with brine, dried with Na2SO4 and evaporated. A oil was obtained which was co-evaporated with toluene and then with diethyl ether before being placed under vacuum for two days. Mass 665 mg (96% yield). NMR (CDCl3): 1.0 (s, 9H), 1.5 (s, 9H), 1.65–1.95 (m, 2H), 3.82 (t, 1H).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US07132416B2 |
|---|
| 출처 데이터셋 | uspto-grants-2006_11 |
|---|
| ORD ID | ord-0448c3b88c404a8db665a533c61a01b8 |
|---|
| 출처 메모 | uspto-grants-2006_11 |
|---|
