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Water → 1-Isothiocyanato-2-(2-methoxyethoxyl)ethane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 1,1'-Thiocarbonyldiimidazole | HCID 80264 | — |
| 反応物 | 2-(2-Methoxyethoxy)ethanamine | HCID 520530 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 1-Isothiocyanato-2-(2-methoxyethoxyl)ethane | HCID 22101683 | 61.2% |
反応手順
To a solution of 2-(2-methoxyethoxyl)ethanamine (0.820 g, 6.88 mmol) in DMF (69 mL) at 0° C. was added dropwise a solution of 1,1′-thiocarbonyldiimidazole (1.349 g, 7.57 mmol) in 21 mL of DMF. The mixture was warmed to RT and stirred for 90 min. The mixture was poured into water (130 mL) and extracted with Et2O (70 mL). The Et2O layer was washed with water, dried over Na2SO4, and filtered. The filtrate was concentrated in vacuo (325 torr, bath temp: 24° C.) to afford 1-isothiocyanato-2-(2-methoxyethoxyl)ethane (0.678 g, 4.21 mmol, 61% yield) as a yellow oil. The crude material was used in next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09394297B2 |
| 出典データセット | uspto-grants-2016_07 |
| ORD ID | ord-b67a0272595a47ff8821def90437bce1 |
| 出典メモ | uspto-grants-2016_07 |