참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 1,1-Dichloroethane | HCID 6365 | — |
| 반응물 | Aluminum(III) Chloride | HCID 6451240 | — |
| 반응물 | 5-Chloromethoxy-4-hydroxy-2-nitrobenzaldehyde | HCID 11424752 | — |
| 용매 | Pyridine | HCID 1049 | — |
| 생성물 | 4,5-Dihydroxy-2-nitrobenzaldehyde | HCID 3782344 | 68.1% |
반응 단계
To a stirred, cooled (0° C.) dispersion of 1.52 g (0.00658 mol) of 5-chloromethoxy-4-hydroxy-2-nitrobenzaldehyde (10), 1 g AlCl3, and 10 ml dry dichloroethane, 2.4 ml of dry pyridine are added. During addition, the reaction mixture is protected from atmospheric moisture, and the temperature is kept below 35° C. When addition is complete, the temperature is raised to 47° C., and maintained for 18 hours. 6N HCl is added, keeping the temperature at 30°-35° C., until the mixture is acidic to Congo Red indicator paper. The acidic solution is extracted with diethyl ether, and the combined ether extracts are dried over Na2SO4. After filtration, the ether is removed at reduced pressure, giving 0.82 g (68%) of (1): mp 201°-202°° C.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 특허 번호 | US04595765 |
|---|
| 출처 데이터셋 | uspto-grants-1986_06 |
|---|
| ORD ID | ord-23064ba024c24eb897ac24e7430ddb49 |
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| 출처 메모 | uspto-grants-1986_06 |
|---|
