Sulfuric Acid → 2,5-Dibromobenzene-1,4-dicarbaldehyde

HRID 580379노트

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HRID 580379 반응식
[Br:1][C:2]1[CH:7]=[C:6]([CH:8](OC(=O)C)[O:9]C(=O)C)[C:5]([Br:17])=[CH:4][C:3]=1[CH:18](OC(=O)C)[O:19]C(=O)C.S(=O)(=O)(O)O>C(O)C.O>[Br:1][C:2]1[CH:7]=[C:6]([CH:8]=[O:9])[C:5]([Br:17])=[CH:4][C:3]=1[CH:18]=[O:19]

참가 물질

5

반응물 2

HCID 1118Sulfuric AcidHCID 13930751HCID 13930751, 화합물

생성물 1

HCID 123535442,5-Dibromobenzene-1,4-dicarbaldehyde수율 87%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

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온도
-10 °C

실험 절차

Unpurified 2,5-dibromo-α,α,α',α'-tetraacetoxy-1,4-xylene (60.5 g, 0.122 mole) was dissolved with stirring in three liters of hot ethanol. Then 450 ml of water was added followed by 75 ml of concentrated sulfuric acid which was added very slowly. After being allowed to reflux for an hour, the reaction mixture was diluted with 900 ml of hot water. Cooling overnight at -10° C. resulted in the recrystallization of 30.9 g (87% yield) of 2,5-dibromoterephthalaldehyde, mp 184°-189° C. (lit 189°-190.5° C.) which was isolated by filtration.

후처리

  1. additionwas added very slowly
  2. temperatureto reflux for an hour

출처 및 근거

ORD 기록
ord-a3ac255917f14e9590b1e52d0854c24b
출처 데이터셋
uspto-grants-1988_06
특허 번호
US04752642

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