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Acetonitrile → 10-[3-(aminomethyl)-1-pyrrolidinyl]-9-fluoro-2,3-dihydro-methyl-7-oxo-7H-pyrido[1,2,3-de]-1,4-benzoxazine-6-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetonitrile | HCID 6342 | — |
| 反応物 | 8,9-Difluoro-3-methyl-6-oxo-2,3-dihydro-6H-1-oxa-3a-aza-phenalene-5-carboxylic acid | HCID 534278 | — |
| 反応物 | 3-Pyrrolidinemethanamine | HCID 5068775 | — |
| 生成物 | 10-[3-(aminomethyl)-1-pyrrolidinyl]-9-fluoro-2,3-dihydro-methyl-7-oxo-7H-pyrido[1,2,3-de]-1,4-benzoxazine-6-carboxylic acid | HCID 70418225 | — |
反応手順
0.75 g (0.27 mmole) of 9,10-difluoro-2,3-dihydro3-methyl-7-oxo-7H-pyrido[1,2,3-de]-1,4-benzoxazine-6-carboxylic acid, 40 ml acetonitrile, and 0.80 g (8.0 mmole) of 3-pyrrolidinemethanamine were refluxed overnight. The solvent was removed at reduced pressure and the residue titurated with 40 ml of ethanol/ether (1:1), to give 0.90 g of 10-[3-(aminomethyl)-1-pyrrolidinyl]-9-fluoro-2,3-dihydro- methyl-7-oxo-7H-pyrido[1,2,3-de]-1,4-benzoxazine-6-carboxylic acid, mp 213°-216° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04771054 |
| 出典データセット | uspto-grants-1988_09 |
| ORD ID | ord-23b85bad7c614b4d9fbedc7ee3c99edd |
| 出典メモ | uspto-grants-1988_09 |