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

HRID 1982219

反応式

HRID 1982219 の反応式
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

参加物

6

反応物 4

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

生成物 1

HCID 37823444,5-Dihydroxy-2-nitrobenzaldehyde収率 68.1%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

反応条件

温度
47 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-23064ba024c24eb897ac24e7430ddb49
出典データセット
uspto-grants-1986_06
特許番号
US04595765

関連ノート

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