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1-Phenethylamine, (+)- → (R)-chroman-2-carboxylic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 1-Phenethylamine, (+)- | HCID 643189 | — |
| 反応物 | 3,4-dihydro-2H-1-benzopyran-2-carboxylic acid | HCID 2723665 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | (R)-chroman-2-carboxylic acid | HCID 6933107 | 13.4% |
反応手順
A solution of (+)-(R)-α-methylbenzylamine (0.37 mol) in ethanol (100 ml) was added to a solution of 3,4-dihydro-2H-1-benzopyran-2-carboxylic acid (0.36 mol) in ethanol (200 ml). The mixture was allowed to crystallize out. The precipitate was filtered off and dried. The residue was crystallized 4 times from ethanol. The precipitate was filtered off and dried. The residue was taken up in water, treated with HCl 10% and extracted with diethyl ether. The organic layer was separated, dried, filtered and the solvent was evaporated, yielding 8.6 g of (−)-(R)-3,4-dihydro-2H-1-benzopyran-2-carboxylic acid (mp. 85.5° C., [α]D20=−6.7° (c=100 mg/10 ml in methanol)) (interm. 1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06852714B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-d04c9a7e0b3c4d64ad8c599e824636af |
| 出典メモ | uspto-grants-2005_02 |