Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
4-Bromobenzaldehyde → 4-(4-Bromo-benzylamino)-2-hydroxy-benzoic acid methyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | 4-Bromobenzaldehyde | HCID 70741 | — |
| 반응물 | Methyl p-aminosalicylate | HCID 77787 | — |
| 반응물 | Sodium Bicarbonate | HCID 516892 | — |
| 반응물 | Sodium triacetoxyborohydride | HCID 5049666 | — |
| 용매 | 1,2-Dichloroethane | HCID 11 | — |
| 용매 | Acetic Acid | HCID 176 | — |
| 용매 | Water | HCID 962 | — |
| 생성물 | 4-(4-Bromo-benzylamino)-2-hydroxy-benzoic acid methyl ester | HCID 58685863 | 58% |
반응 단계
To a solution of 4-amino-2-hydroxy benzoic acid methyl ester (836 mg; 5 mmol) and 4-bromobenzaldehyde (926 mg; 5 mmol) in 1 M HOAc in 1,2-dichloroethane (5 mL) was added at once NaBH(OAc)3 (1.49 g; 7 mmol) and the reaction mixture was stirred at room temperature overnight. Water (25 mL) was added and the inhomogeneous mixture was neutralized using solid NaHCO3. The organic layer was isolated, dried, evaporated to dryness and recrystallised from isopropyl ether/dichloromethane/heptane to yield 970 mg (58%) of a yellow solid. NMR and GC-MS in accordance with structure.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US07741352B2 |
| 출처 데이터셋 | uspto-grants-2010_06 |
| ORD ID | ord-27627b1c3a684507b64c67ddba27ff91 |
| 출처 메모 | uspto-grants-2010_06 |