化工社化工社 化学情報印刷レポート · 研究参考用
Sodium Hydroxide → N-(cyclohexylmethyl)-2,2-diethoxyethanamine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | Cyclohexanecarboxaldehyde | HCID 16275 | — |
| 反応物 | 2,2-Diethoxyethylamine | HCID 69524 | — |
| 反応物 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 溶媒 | 2-Methyltetrahydrofuran | HCID 7301 | — |
| 生成物 | N-(cyclohexylmethyl)-2,2-diethoxyethanamine | HCID 60052150 | — |
反応手順
To a mixture of 2,2-diethoxyethylamine (209 mL, 1.43 mol) and MeTHF (1050 L) was added cyclohexanecarbaldehyde (107 mL, 0.89 mol). The reaction mixture was stirred for 30 min at room temperature and cooled to 0° C. Sodium triacetoxyborohydride (378 g, 1.79 mol) was added over 40 min and the reaction mixture was stirred for 2 h and cooled to 0° C. 1 M NaOH (1 L) was added. The organic layer was washed with brine in water (1:1, 2×1 L) and the volume was reduced to ˜20%. MeTHF (1 L) was added and the volume reduced to ˜20%. The solution of the crude title intermediate was used directly in the next step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08536335B2 |
| 出典データセット | uspto-grants-2013_09 |
| ORD ID | ord-2ae19a871ca64856a3312bef045f65b0 |
| 出典メモ | uspto-grants-2013_09 |