2-Chloro-7-methoxynaphthalene-1,4-dione → HCID 13455828、化合物

HRID 569231ノート

反応式

HRID 569231 の反応式
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

参加物

3

反応物 1

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

生成物 1

HCID 13455828HCID 13455828、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

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%).

後処理

  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%)

出典と根拠

ORDレコード
ord-fd71f582541246d3b3985519e0413735
出典データセット
uspto-grants-1988_03
特許番号
US04731468

反応ノート

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