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Triethylamine → (S)-1-Boc-3-isopropylpiperazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2-(tert-Butoxycarbonyloxyimino)-2-phenylacetonitrile | HCID 93865 | — |
| 反応物 | (S)-2-Isopropylpiperazine | HCID 15023839 | — |
| 反応物 | Dichloromethane methanol | HCID 21226129 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | 1,4-Dioxane | HCID 31275 | — |
| 生成物 | (S)-1-Boc-3-isopropylpiperazine | HCID 24820348 | 74.9% |
反応手順
341 mg (2.66 mmol) 2-(S)-Isopropyl-piperazine (84) and 657 mg (2.67 mmol, 1.00 eq.) BOC-ON© (2-(tert-Butoxycarbonyloxyimino)-2-phenylacetonitrile) were dissolved in 20 ml 1,4-dioxane and 20 ml water. After adding 2.04 ml (14.64 mmol, 5.50 eq.) triethylamine the solution was stirred at r.t. for 24 h. Then the mixture was added to water and extracted with EtOAc. The comb. org. fractions were washed with brine, dried over Na2SO4 and evaporated. Column chromatography (CH2Cl2/MeOH (3+1)) yielded 454.9 mg (1.99 mmol, 74.90%) 3-(S)-Isopropyl-piperazine-1-carboxylic acid tert-butyl ester (85) as a clear oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06858600B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-d95c0cf80dc140a8b7f0457decee3580 |
| 出典メモ | uspto-grants-2005_02 |