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Hydrazine hydrate (1:1) → tert-butyl N-[(hydrazinecarbonyl)methyl]carbamate
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | N-Boc-glycine methyl ester | HCID 637609 | — |
| 生成物 | tert-butyl N-[(hydrazinecarbonyl)methyl]carbamate | HCID 2735639 | — |
反応手順
To a stirred solution of methyl (tert-butyloxycarbonyl)glycinate (8.54 g, 45.1 mmol) was added hydrazine hydrate (4.4 mL, 90.5 mmol) and the reaction was heated under reflux for 16 hours. The solvent was removed in vacuo and the residue partitioned between dichloromethane (100 mL) and water (100 mL). The phases were separated, the aqueous phase evaporated in vacuo to low volume and extracted with 5% methanol/dichloromethane (2×100 mL) The organic extracts were combined, dried over magnesium sulfate and concentrated in vacuo to give the product as a white crystalline solid, 5.27 g (62%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07456170B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-6cad0116a93643169fa517c01313d7c6 |
| 出典メモ | uspto-grants-2008_11 |