Methanol → 1,5-Dimethoxynaphthalene

HRID 1057215

반응식

HRID 1057215 반응식
[C:1](#N)C.CO.S([O:11][CH3:12])(OC)(=O)=O.O[C:14]1[C:23]2[C:18](=[C:19]([OH:24])[CH:20]=[CH:21][CH:22]=2)[CH:17]=[CH:16][CH:15]=1>[OH-].[Na+].C(Cl)(Cl)Cl.CN(C)C=O>[CH3:1][O:24][C:19]1[C:18]2[C:23](=[C:14]([O:11][CH3:12])[CH:15]=[CH:16][CH:17]=2)[CH:22]=[CH:21][CH:20]=1

참가 물질

8

반응물 4

HCID 887MethanolHCID 6342AcetonitrileHCID 6497Dimethyl SulfateHCID 67491,5-Dihydroxynaphthalene

생성물 1

HCID 2525271,5-Dimethoxynaphthalene

시약·촉매·용매 3

HCID 6212Chloroform용매HCID 6228Dimethylformamide용매HCID 14798Sodium Hydroxide용매2회

실험 절차

1,4,5,8-tetramethoxynaphthalene (3) is synthesized from 1,5-dihydroxynaphthalene (2) as a starting material through a known three-phase reaction, and then 1,4,5,8-tetramethoxynaphthalene (3) is demethylated to produce 5,8-dimethoxy-1,4-naphtoquinone(4) as a synthesis intermediate. A detailed synthesis method is disclosed in cited references presented in the reaction schemes above, and a solvent used herein may be a solvent that does not adversely affect the reaction, and examples of such a solvent are sodium hydroxide, acetonitrile, anhydrous methanol, N, N-dimethylformamide, and chloroform. The initial methylation is performed in such a manner that dimethyl sulfate is dropped to 1,5-dihydroxynaphthalene dissolved in sodium hydroxide in the presence of a nitrogen gas for 1 hour and the reaction was performed for 2 hours. The reaction product is re-crystallized with benzene to produce 1,5-dimethoxynaphthalene.

후처리

  1. customA detailed synthesis method
  2. custompresented in the reaction schemes above, and a solvent
  3. customThe reaction product is re-crystallized with benzene

출처 및 근거

ORD 기록
ord-880d6cc55fed4c0ab68de442be23da80
출처 데이터셋
uspto-grants-2016_07
특허 번호
US09400281B2

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