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Diphenyl Ether → 9-Methoxy-2-methyl-7h-furo[3,2-g]chromen-7-one

HRID 1448518
ノート
印刷プレビュー

反応式

HRID 1448518 の反応式
[CH3:1][CH:2]1[O:17][C:5]2=[C:6]([O:15][CH3:16])[C:7]3[O:12][C:11](=[O:13])[CH:10]=[CH:9][C:8]=3[CH:14]=[C:4]2[CH2:3]1.C1(OC2C=CC=CC=2)C=CC=CC=1>[Pd]>[CH3:16][O:15][C:6]1[C:7]2[O:12][C:11](=[O:13])[CH:10]=[CH:9][C:8]=2[CH:14]=[C:4]2[CH:3]=[C:2]([CH3:1])[O:17][C:5]=12
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 7583Diphenyl EtherHCID 203802232-methyl-9-methoxy-2,3-dihydro-7H-furo[3,2-g][1]benzopyran-7-one

生成物 1

HCID 1653069-Methoxy-2-methyl-7h-furo[3,2-g]chromen-7-one

試薬・触媒・溶媒 1

HCID 23938Palladium触媒

実験手順

To a solution of 0.70 g. (3.02 mmoles) of 2-methyl-9-methoxy-2,3-dihydro-7H-furo[3,2-g][1]benzopyran-7-one in 15 ml. of diphenyl ether was added 0.70 g. of 10% Pd/C. The mixture was heated under reflux for 6.0 hours, cooled, and filtered over Celite (washing with methanol). The methanol was removed from the filtrate by rotary evaporation, and the remaining solution of the product in diphenyl ether was diluted with 200 ml. of pet. ether. After standing overnight, the solid which separated was filtered off and washed with pet. ether to yield 9-methoxy-2-methyl-7H-furo[3,2-g][1]benzopyran-7-one. Recrystallization from ethanol afforded an analytical sample, mp 149°-150°.

後処理

  1. temperatureThe mixture was heated
  2. temperatureunder reflux for 6.0 hours
  3. temperaturecooled
  4. filtrationfiltered over Celite (washing with methanol)
  5. customThe methanol was removed from the filtrate by rotary evaporation
  6. additionthe remaining solution of the product in diphenyl ether was diluted with 200 ml
  7. customthe solid which separated
  8. filtrationwas filtered off
  9. washwashed with pet. ether

出典と根拠

ORDレコード
ord-7cd132baa8c945c6b94a061603f711fe
出典データセット
uspto-grants-1979_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04180659

反応ノート

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