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Dimethylformamide → (+/-)-4-[[(3,4-dihydro-2H-1-benzopyran-2-yl)methyl](phenylmethyl) amino]-butanenitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethylformamide | HCID 6228 | — |
| 反応物 | 4-Bromobutyronitrile | HCID 21412 | — |
| 反応物 | Benzyl-chroman-2-ylmethyl-amine; oxalic acid | HCID 10753388 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | (+/-)-4-[[(3,4-dihydro-2H-1-benzopyran-2-yl)methyl](phenylmethyl) amino]-butanenitrile | HCID 21460889 | 69.6% |
反応手順
A mixture of 12.5 g of 3,4-dihydro-N-(phenylmethyl)-2H-1-benzopyran-2-methanamine, 9 g of 4-bromobutanenitrile, 200 ml of N,N-dimethylformamide and 10 ml of N,N-diethylethanamine was stirred for 72 hour at room temperature. The reaction mixture was evaporated and the residue was partitioned between 1,1'-oxybisethane and water. The organic layer was separated, dried, filtered and evaporated, yielding 11 g (68.7%) of (±)-4-[[(3,4-dihydro-2H-1-benzopyran-2-yl)methyl](phenylmethyl) amino]-butanenitrile (interm. 53).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05624952 |
| 出典データセット | uspto-grants-1997_04 |
| ORD ID | ord-f31c99b19d4442d2a302c1cf4cb988b9 |
| 出典メモ | uspto-grants-1997_04 |