2-Chloro-7-methoxynaphthalene-1,4-dione → HCID 13455828, 화합물

HRID 569231노트

반응식

HRID 569231 반응식
Cl[C:2]1[C:11](=[O:12])[C:10]2[C:5](=[CH:6][CH:7]=[C:8]([O:13][CH3:14])[CH:9]=2)[C:4](=[O:15])[CH:3]=1>O1CCCC1>[OH:15][C:4]1[C:2]2[C:11](=[O:12])[C:10]3[C:5](=[CH:6][CH:7]=[C:8]([O:13][CH3:14])[CH:9]=3)[C:4](=[O:15])[C:3]=2[CH:11]=[C:10]2[C:5]=1[CH2:6][CH2:7][C:8](=[O:13])[CH2:9]2

참가 물질

3

반응물 1

HCID 128295782-Chloro-7-methoxynaphthalene-1,4-dione

생성물 1

HCID 13455828HCID 13455828, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

A solution of the keten acetal VII (2.5 g; 8.9 mmol) in tetrahydrofuran (THF) (3 ml) is added dropwise at 0° C. to a solution of 3-chloro-6-methoxy-1,4-naphthoquinone (1.9 g; 8.6 mmol) in THF (20 ml). The reaction medium is stirred overnight at ambient temperature. After evaporation of the solvent, the solid obtained is added slowly to a solution of HF (25 ml)-SbF5 (5 ml) at -40° C. in a Teflon flask. The mixture is kept at -40° C. for 20 minutes and then poured slowly into 500 ml of a water/ice mixture. After extraction with methylene chloride, the organic phase is washed with water, dried over sodium sulfate and then evaporated. The tetracyclic ketone is purified by chromatography under pressure (eluent: CH2Cl2) (1.11 g; 40%).

후처리

  1. customAfter evaporation of the solvent
  2. customthe solid obtained
  3. waitThe mixture is kept at -40° C. for 20 minutes
  4. extractionAfter extraction with methylene chloride
  5. washthe organic phase is washed with water
  6. dry with materialdried over sodium sulfate
  7. customevaporated
  8. customThe tetracyclic ketone is purified by chromatography under pressure (eluent: CH2Cl2) (1.11 g; 40%)

출처 및 근거

ORD 기록
ord-fd71f582541246d3b3985519e0413735
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04731468

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