Anisole → 1,8-Dihydroxy-2,7-di(4-methoxyphenyl)-4,5-dinitroanthraquinone

HRID 1789324

반응식

HRID 1789324 반응식
[OH:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[C:9]([N+:18]([O-:20])=[O:19])[CH:10]=[CH:11][C:12]=3[OH:17])[C:7](=[O:21])[C:6]=2[C:5]([N+:22]([O-:24])=[O:23])=[CH:4][CH:3]=1.[C:25]1([O:31][CH3:32])[CH:30]=[CH:29][CH:28]=[CH:27][CH:26]=1>B(O)(O)O.S(=O)(=O)(O)O>[OH:1][C:2]1[C:15]2[C:14](=[O:16])[C:13]3[C:8](=[C:9]([N+:18]([O-:20])=[O:19])[CH:10]=[C:11]([C:28]4[CH:29]=[CH:30][C:25]([O:31][CH3:32])=[CH:26][CH:27]=4)[C:12]=3[OH:17])[C:7](=[O:21])[C:6]=2[C:5]([N+:22]([O-:24])=[O:23])=[CH:4][C:3]=1[C:28]1[CH:29]=[CH:30][C:25]([O:31][CH3:32])=[CH:26][CH:27]=1

참가 물질

5

반응물 2

HCID 7519AnisoleHCID 33784401,8-Dinitro-4,5-dihydroxyanthraquinone

생성물 1

HCID 201880501,8-Dihydroxy-2,7-di(4-methoxyphenyl)-4,5-dinitroanthraquinone수율 77.5%

시약·촉매·용매 2

HCID 1118Sulfuric Acid용매HCID 7628Boric Acid용매

반응 조건

온도
0 °C

실험 절차

9.9 g of 1,8-dihydroxy-4,5-dinitroanthraquinone are dissolved in a mixture of 15.6 g of boric acid and 228 g of 100 percent sulphuric acid. The solution obtained is cooled down to -10° to 0° C. and 7.4 g of anisole are added dropwise. The temperature is maintained for a further 1 hour at 0° C. and then the mixture is poured onto 240 g of ice and heated to reflux for 4 hours. The solid is filtered off with suction, washed with water to neutrality and dried at 60° C. 12.6 g of 1,8-dihydroxy-2,7-di(4-methoxyphenyl)-4,5-dinitroanthraquinone, corresponding to a yield of 77% of theory, are obtained.

후처리

  1. customThe solution obtained
  2. temperatureis cooled down to -10° to 0° C.
  3. temperatureheated
  4. temperatureto reflux for 4 hours
  5. filtrationThe solid is filtered off with suction
  6. washwashed with water to neutrality
  7. customdried at 60° C

출처 및 근거

ORD 기록
ord-189ddf3bf8b14151ae66f2b2feefb8e0
출처 데이터셋
uspto-grants-1987_08
특허 번호
US04689171

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