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Hydrazine hydrate (1:1) → [2-(2-Methoxyethoxy)-ethyl]-hydrazine
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 | 1-Bromo-3,6-dioxaheptane | HCID 123532 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | [2-(2-Methoxyethoxy)-ethyl]-hydrazine | HCID 18959038 | 85% |
反応手順
To a solution of hydrazine monohydrate (44.0 mL, 1.00 mol) in ethanol (75 mL) at 0° C. in an ice-water bath was added 1-(2-bromoethoxy)-2-methoxyethane (13.6 mL, 0.100 mol) drop-wise over 20 minutes. The reaction was then allowed to warm to room temperature and stir for 5 minutes and then heated to 40° C. in a preheated oil bath for 12 hours. The reaction was then cooled to room temperature and concentrated to remove the ethanol. The remaining aqueous layer was extracted with methylene chloride (2×100 mL) and diethyl ether (2×100 mL). The organic layers were combined and dried over anhydrous Na2SO4, filtered and concentrated to provide [2-(2-methoxyethoxy)-ethyl]-hydrazine as a light yellow oil (10.29 g, 85%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07728029B2 |
| 出典データセット | uspto-grants-2010_06 |
| ORD ID | ord-1759ce57e6de40e986407126f2e925cc |
| 出典メモ | uspto-grants-2010_06 |