Hydrochloric Acid → 4,5-Dihydroxy-2-nitrobenzaldehyde

HRID 1982219

반응식

HRID 1982219 반응식
ClC[O:3][C:4]1[C:5]([OH:15])=[CH:6][C:7]([N+:12]([O-:14])=[O:13])=[C:8]([CH:11]=1)[CH:9]=[O:10].[Al+3].[Cl-].[Cl-].[Cl-].ClC(Cl)C.Cl>N1C=CC=CC=1>[OH:15][C:5]1[C:4]([OH:3])=[CH:11][C:8]([CH:9]=[O:10])=[C:7]([N+:12]([O-:14])=[O:13])[CH:6]=1

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 63651,1-DichloroethaneHCID 6451240Aluminum(III) ChlorideHCID 114247525-Chloromethoxy-4-hydroxy-2-nitrobenzaldehyde

생성물 1

HCID 37823444,5-Dihydroxy-2-nitrobenzaldehyde수율 68.1%

시약·촉매·용매 1

HCID 1049Pyridine용매

반응 조건

온도
47 °C

실험 절차

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.

후처리

  1. additionare added
  2. additionDuring addition
  3. customis kept below 35° C
  4. additionWhen addition
  5. temperaturemaintained for 18 hours
  6. customat 30°-35° C.
  7. extractionThe acidic solution is extracted with diethyl ether
  8. dry with materialthe combined ether extracts are dried over Na2SO4
  9. filtrationAfter filtration
  10. customthe ether is removed at reduced pressure

출처 및 근거

ORD 기록
ord-23064ba024c24eb897ac24e7430ddb49
출처 데이터셋
uspto-grants-1986_06
특허 번호
US04595765

연결된 노트

불러오는 중…