참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | 2-Methyl-2-butanol | HCID 6405 | — |
| 반응물 | Chloride 2-chloropyridinium 1-oxide | HCID 88478 | — |
| 반응물 | N-BOC-ethylenediamine | HCID 187201 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | HCID 178453672 | HCID 178453672 | 89.3% |
반응 단계
A mixture of mono-Boc-1,2-ethylenediamine (5.83 g, 36.39 mmole), 2-chloropyridine-N-oxide hydrochloride (7.25 g, 43.67 mmole), NaHCO3 (15.29 g, 182 mmole), and tert-amyl alcohol (36 mL) was heated at reflux. After 47 hr, the dark brown mixture was cooled, diluted with CH2Cl2 (100 mL), and suction filtered to remove insoluble materials. The filtrate was concentrated and reconcentrated from toluene. Silica gel chromatography (10% MeOH/CHCl3) gave impure title compound (8.23 g, 89%) as a yellow solid which was used without further purification: TLC (10% MeOH/CHCl3) Rf 0.42; 1H NMR (250, CDCl3) δ 8.16 (dd, J=6.5, 1.3 Hz, 1 H), 7.05-7.30 (m, 2 H), 6.68 (br d, J=8.6 Hz, 1 H), 6.50-6.65 (m, 1 H), 5.70-5.95 (m, 1 H), 3.35-3.60 (m, 4 H), 1.44 (s, 9 H); MS (ES) m/e 254 (M+H)+.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US06008213 |
|---|
| 출처 데이터셋 | uspto-grants-1999_12 |
|---|
| ORD ID | ord-14ee808ca3384c56bd282f6d7041f04e |
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| 출처 메모 | uspto-grants-1999_12 |
|---|
