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3-Hydroxy-2,2-dimethylpropionaldehyde → HCID 22573178、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 3-Hydroxy-2,2-dimethylpropionaldehyde | HCID 11699 | — |
| 反応物 | HCID 10330538 | HCID 10330538 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | HCID 22573178 | HCID 22573178 | 21.5% |
反応手順
The reaction is run similar to the preparation in Example 11. To a MeOH solution of 4 Å powdered molecular sieves (0.35 g) under argon is added 3-amino-6,7-dimethoxyquinoline (0.32 g, 1.6 mmol) and 2,2-dimethyl-3-hydroxypropionaldehyde (0.19 g, 1.9 mmol). The product mixture is chromatographed (3% MeOH/CHCl3) to afford 0.10 g of material which is partitioned between CH2Cl2/10% NaOH. The organic layer is washed with 10% NaOH, H2O, and brine, then dried (MgSO4), and recrystallized from EtOAc/hexanes to provide a light-orange solid (m.p. 170-173.5° C.). Anal. Calcd. for C16H22N2O3: C, 66.18; H, 7.64; N, 9.65; Found: C, 66.11; H, 7.49; N, 9.33.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06852712B2 |
| 出典データセット | uspto-grants-2005_02 |
| ORD ID | ord-6c227764ca054552b7a5977f95fc5ec6 |
| 出典メモ | uspto-grants-2005_02 |