참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Dichloromethane | HCID 6344 | — |
| 반응물 | Diisopropylethylamine | HCID 81531 | — |
| 반응물 | O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborate | HCID 2733207 | — |
| 반응물 | 4-(tert-Butoxycarbonyl)morpholine-3-carboxylic acid | HCID 2760133 | — |
| 생성물 | Diisopropylethylamine | HCID 81531 | — |
| 생성물 | Methyl D-alaninate hydrochloride | HCID 11182647 | — |
| 생성물 | (3R)-3-methyltetrahydro-2H-pyrazino[1,2-a]pyrazine-1,4(3H,6H)-dione | HCID 59215897 | — |
반응 단계
To a solution of N-boc-morpholine-3-carboxylic acid (2 g, 9.379 mmol) in 60 mL of dichloromethane and was added TBTU (3.313 g, 10.32 mmol) and diisopropylethyl amine (1.96 mL, 11.25 mmol). The reaction was stirred for 30 min. In the meantime, a solution of D-alanine methyl ester hydrochloride (1.93 g, 18.76 mmol) and diisopropylethylamine (3.27 mL, 18.76 mmol) in 20 mL of dichloromethane was prepared and finally added to the reaction mixture. The reaction was left stirring at room temperature for 2 h. UPLC-MS analysis showed the expected product (peak at 0.60 min, m/z=317 (M+1), 261 (M−t-Bu+1), 217 (M−Boc+1)). The reaction was diluted with dichloromethane and extracted with sat. NaHCO3, dried (Na2SO4), and the solvent removed. The crude (5.56 g) was taken to the next step without further purification.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US08097618B2 |
|---|
| 출처 데이터셋 | uspto-grants-2012_01 |
|---|
| ORD ID | ord-fca0426383df493bb055573c88de7bea |
|---|
| 출처 메모 | uspto-grants-2012_01 |
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