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Ethyl Acetate → 4-(3-Amino-5-chloro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 4-(5-Chloro-3-nitro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester | HCID 59548752 | — |
| 触媒 | Platinum sulfide (PtS) | HCID 82861 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 4-(3-Amino-5-chloro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester | HCID 59548867 | 80% |
反応手順
A round bottom flask is charged with 5% platinum sulfide on carbon (0.20 g, 0.039 mmol). The flask was evacuated and refilled with argon three times. To the flask is added 4-(5-chloro-3-nitro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester (2.80 g, 8.17 mmol) as a solution in a 1:1 mixture of ethyl acetate:methanol (100 mL). The mixture is placed under an atmosphere of hydrogen and stirred overnight at room temperature. The mixture is filtered through a pad of diatomaceous earth and concentrated under reduced pressure to provide 2.0 g of 4-(3-amino-5-chloro-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester as a dark solid in 80% yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08362249B2 |
| 出典データセット | uspto-grants-2013_01 |
| ORD ID | ord-8b8d07f68af74df58478088be04b392d |
| 出典メモ | uspto-grants-2013_01 |