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Potassium Iodide → 4,4-dimethyl-pyrazolidine N,N'-dicarboxylic acid di-tert-buty1 ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Di-tert-butyl bicarbamate | HCID 85431 | — |
| 反応物 | Neopentyl glycol dimethylsulfate | HCID 299203 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4,4-dimethyl-pyrazolidine N,N'-dicarboxylic acid di-tert-buty1 ester | HCID 54489555 | 2% |
反応手順
41.8 g of hydrazine-N,N'-dicarboxylic acid di-tert-butyl ester, 74.5 g of potassium carbonate, 52.0 g of 2,2-dimethyl-1,3-propanediol dimethanesulfonate and 2.0 g of potassium iodide are stirred for 48 hours at 120°-130° C. in 360 ml of N,N-dimethylformamide. The reaction mixture is then concentrated; diethyl ether is added and the organic phase is washed with water. Mter drying over sodium sulfate, the reaction mixture is concentrated and purified by means of column chromatography to yield 1.1 g of the desired product, 4,4-dimethyl-pyrazolidine-N,N'-dicarboxylic acid di-tert-butyl ester, in the form of white crystals.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05416065 |
| 出典データセット | uspto-grants-1995_05 |
| ORD ID | ord-d11c6c925c1348ed84d5539cdd66929d |
| 出典メモ | uspto-grants-1995_05 |