참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-Methyl-2-butanol | HCID 6405 | — |
| 반응물 | 3-Amino-1-propanol | HCID 9086 | — |
| 반응물 | 2-Chloropyridine oxide | HCID 75465 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 용매 | Chloroform methanol | HCID 21584188 | — |
| 생성물 | HCID 178526251 | HCID 178526251 | 93% |
반응 단계
A mixture of 2-chloropyridine-N-oxide (16.6 g, 0.1 mole), 3-amino-1-propanol (15.3 mL, 0.2 mole), NaHCO3 (42 g, 0.5 mole), and tert-amyl alcohol (100 mL) was heated to reflux. After 21 hr, the reaction was cooled, diluted with CH2Cl2 (300 mL), and suction filtered to remove insoluble materials. The filtrate was concentrated and reconcentrated from toluene to leave a yellow oil. Silica gel chromatography (20% MeOH/CHCl3) gave the title compound (15.62 g, 93%) as a yellow solid: TLC (20% MeOH/CHCl3) Rf 0.48; 1H NMR (250, CDCl3) δ 8.07 (dd, J=6.6, 1.2 Hz, 1 H), 7.34 (br t, 1 H), 7.10-7.30 (m, 1 H), 6.64 (dd, J=8.5, 1.4 Hz, 1 H), 6.40-6.60 (m, 1 H), 4.49 (br s, 1 H), 3.65-3.90 (m, 2 H), 3.35-3.60 (m, 2 H), 1.75-2.00 (m, 2 H); MS (ES) m/e 169 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06008213 |
|---|
| 출처 데이터셋 | uspto-grants-1999_12 |
|---|
| ORD ID | ord-b6960fd79dce4bc0b5a57ced0b12d413 |
|---|
| 출처 메모 | uspto-grants-1999_12 |
|---|
