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L-Proline → (S)-1,2,3,11a-tetrahydro-6-methyl-5H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11(10H)-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | L-Proline | HCID 145742 | — |
| 反応物 | 5-methyl-2,4-dihydro-1H-3,1-benzoxazine-2,4-dione | HCID 10487522 | — |
| 溶媒 | Dimethyl Sulfoxide | HCID 679 | — |
| 生成物 | (S)-1,2,3,11a-tetrahydro-6-methyl-5H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11(10H)-dione | HCID 13891432 | — |
反応手順
A solution of 13.6 g (0.0768 mol) of 6-methylisatoic acid anhydride and 8.8 g (0.0768 mol) of L-proline is heated at 110° C. for 1 hour in 75 ml of dimethyl sulphoxide. Subsequently, the mixture is evaporated to dryness in a high vacuum and the residue is recrystallised from ethyl acetate with the addition of active carbon. There is obtained (S)-1,2,3,11a-tetrahydro-6-methyl-5H-pyrrolo[2,1-c][1,4]benzodiazepine-5,11(10H)-dione of melting point 212°-214° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04346032 |
| 出典データセット | uspto-grants-1982_08 |
| ORD ID | ord-3c83a733826840d689109ed1ab7abf7e |
| 出典メモ | uspto-grants-1982_08 |