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2-(cis-2,6-Dimethyl-1-piperidinyl)ethanamine → cis-(+-)-N-(2-(2,6-Dimethyl-1-piperidinyl)ethyl)-2-oxo-3-hydroxy-1-pyrrolidineacetamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-(cis-2,6-Dimethyl-1-piperidinyl)ethanamine | HCID 783702 | — |
| 反応物 | ethyl (R/S)-2-(3-hydroxy-2oxo-1-pyrrolidinyl)acetate | HCID 13385945 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | cis-(+-)-N-(2-(2,6-Dimethyl-1-piperidinyl)ethyl)-2-oxo-3-hydroxy-1-pyrrolidineacetamide | HCID 3069833 | — |
反応手順
4.5 g of ethyl (R/S)-2-(3-hydroxy-2-oxo-1-pyrrolidinyl)-acetate are heated to 100° for 3.5 hours under nitrogen with 7.1 g of cis-2-(2,6-dimethyl-1-piperidinyl)ethylamine. Thereafter, diethyl ether is added thereto, the mixture is stirred, filtered and the filter residue (6.5 g) is chromatographed on 30 g of silica gel (granular size 0.2-0.5 mm). The (R/S)-cis-N-pi [2-(2,6-dimethyl-1-piperidinyl)-ethyl]-2-(3-hydroxy-2-oxo-1-pyrrolidinyl)acetamide which is eluted with methylene chloride and methanol has a melting point of 131°-132° after recrystallization from ethyl acetate.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05034402 |
| 出典データセット | uspto-grants-1991_07 |
| ORD ID | ord-1d8dd31cb0cd49ecac8b928c4365234a |
| 出典メモ | uspto-grants-1991_07 |