Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Tetrahydrofuran → 4,5-Diamino-3-chloro-2-phenylamino-benzoic acid methyl ester
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Tetrahydrofuran | HCID 8028 | — |
| 반응물 | Ammonium Chloride | HCID 25517 | — |
| 반응물 | Ethanol, mixt. with methanol | HCID 18681192 | — |
| 반응물 | 4-Amino-3-chloro-5-nitro-2-phenylamino-benzoic acid methyl ester | HCID 85868196 | — |
| 촉매 | Zinc | HCID 23994 | — |
| 용매 | Water | HCID 962 | — |
| 용매 | Tetrahydrofurane dichloromethane | HCID 21919333 | — |
| 생성물 | 4,5-Diamino-3-chloro-2-phenylamino-benzoic acid methyl ester | HCID 85868198 | 70.8% |
반응 단계
4-Amino-3-chloro-5-nitro-2-phenylamino-benzoic acid methyl ester 5c (0.50 g, 1.55 mmol) is dissolved into 2:1 EtOH/MeOH (15.5 mL). Saturated aqueous NH4Cl (15 mL), Zn powder (1.02 g, 15.6 mmol), and THF (10 mL) are added. After stirring for 20 hours, the reaction mixture is diluted with CH2Cl2/THF and water. The organic layer is washed with water (3×). The combined organic extracts are dried (Na2SO4) and concentrated under reduced pressure. The solids are triturated with ether to give 0.32 g (70%) clean desired product.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US08193231B2 |
| 출처 데이터셋 | uspto-grants-2012_06 |
| ORD ID | ord-5578053e37d0426f97e5645bfe047a76 |
| 출처 메모 | uspto-grants-2012_06 |