Iodine → HCID 12401704、化合物

HRID 236890ノート

反応式

HRID 236890 の反応式
[C:1](O)(=[O:3])C.CS[CH:7]([OH:19])[C:8]1[O:9][C:10]2[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=2[C:12](=[O:14])[CH:13]=1.II.[CH3:22]O>>[CH3:1][O:3][CH:7]([O:19][CH3:22])[C:8]1[O:9][C:10]2[CH:18]=[CH:17][CH:16]=[CH:15][C:11]=2[C:12](=[O:14])[CH:13]=1

参加物

4

反応物 3

HCID 807IodineHCID 887MethanolHCID 70601480HCID 70601480、化合物

生成物 1

HCID 12401704HCID 12401704、化合物収率 86%

実験手順

A stirred solution of 2-[(methylthio)hydroxymethyl)-4H-1- benzopyran-4-one acetate](2.64 g, 0.01 m) and iodine (1.39 g, 0.01 m) in methanol (50 ml) was refluxed under nitrogen for 6 hours. After cooling, the solvents were removed under reduced pressure. The red-brown oil was dissolved in chloroform and washed three times (30 ml) with aqueous saturated sodium thiosulfate. The chloroform extract was dried over sodium sulfate. Removal of the solvent under reduced pressure gave crude solid product. Recrystallization from isopropyl ether gave yellow crystals (1.9 g, 86%), m.p. 64°-68°.

後処理

  1. temperatureAfter cooling
  2. customthe solvents were removed under reduced pressure
  3. dissolutionThe red-brown oil was dissolved in chloroform
  4. washwashed three times (30 ml) with aqueous saturated sodium thiosulfate
  5. extractionThe chloroform extract
  6. dry with materialwas dried over sodium sulfate
  7. customRemoval of the solvent under reduced pressure
  8. customgave crude solid product
  9. customRecrystallization from isopropyl ether

出典と根拠

ORDレコード
ord-b4026119675d4501b228acc94bfb1628
出典データセット
uspto-grants-1979_06
特許番号
US04158663

反応ノート

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