Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Hydrochloric Acid → 6-[(Tert-butoxy)carbonyl]pyridine-3-carboxylic acid
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | Sodium Hydroxide | HCID 14798 | — |
| 반응물 | 2-Tert-butyl 5-methyl pyridine-2,5-dicarboxylate | HCID 54326310 | — |
| 촉매 | ICE protocol 1 | HCID 56841950 | — |
| 용매 | Tetrahydrofuran | HCID 8028 | — |
| 생성물 | 6-[(Tert-butoxy)carbonyl]pyridine-3-carboxylic acid | HCID 22271447 | 76% |
반응 단계
A mixture of methyl 6-tert-butoxycarbonylnicotinate (1.2 g, 5.06 mmol) in THF (15 ml) and 0.25 N NaOH (40 ml, 10 mol) at an ambient temperature for 0.5 hr. The mixture was poured into ice-1 N HCl (10 ml). The solid was collected, washed with water and air-dried. The crude solid was recrystallized from CHCl3-EtOH-IPE to afford 6-tert-butoxycarbonylnicotinic acid (850 mg, 76%) as needles. IR (KBr) n3095, 1728, 1705 cm−1; 1H-NMR (DMAO-d6) δ 1.63 (s, 9 H), 8.09 (m, 1 H), 8.17 (m, 1 H), 8.42 (dt, J=2.4 and 8.3 Hz, 1 H), 9.21 (t, J=2.4 and 8.8 Hz, 1 H); MS (FAB) m/z 224 (M++1); Anal. Calcd for C29H33N3O6: C, 36.18; H, 3.18; N, 3.84. Found: C, 36.85; H, 3.35; N, 3.79.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07179819B2 |
| 출처 데이터셋 | uspto-grants-2007_02 |
| ORD ID | ord-7757f7804b764518a6dbfa2b2a7862d8 |
| 출처 메모 | uspto-grants-2007_02 |