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Thiophene → methyl N-(2,3-dihydro-3-methyl-1H-inden-1-yl)glycine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Thiophene | HCID 8030 | — |
| 反応物 | Glycine methyl ester | HCID 69221 | — |
| 反応物 | 3-Methyl-indan-1-one | HCID 259560 | — |
| 反応物 | Sodium Formate | HCID 2723810 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | methyl N-(2,3-dihydro-3-methyl-1H-inden-1-yl)glycine | HCID 67861921 | 54.1% |
反応手順
A mixture of 21 parts of 2,3-dihydro-3-methyl-1H-inden-1-one, 25 parts of methyl 2-aminoacetate, 2 parts of a solution of thiophene in methanol 4%, 25 parts of sodium formate and 480 parts of methanol is hydrogenated in a Parr-apparatus and at 50° C. with 5 parts of palladium-on-charcoal catalyst 10%. The reaction mixture is evaporated. The residue is taken up in water and 1,1'-oxybisethane is added. The separated organic layer is extracted with a hydrochloric acid solution 10%. The aqueous layer is made alkaline and the product is extracted with 1,1'-oxybisethane. The combined extracts are dried, filtered and evaporated, yielding 19 parts (54.1%) of methyl N-(2,3-dihydro-3-methyl-1H-inden-1-yl)glycine as a residue.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05246915 |
| 出典データセット | uspto-grants-1993_09 |
| ORD ID | ord-e1764cad45a24269bfb95b0d00a282b2 |
| 出典メモ | uspto-grants-1993_09 |