Iodine → HCID 12401704, 화합물

HRID 236890노트

반응식

HRID 236890 반응식
[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

참가 물질

4

반응물 3

HCID 807IodineHCID 887MethanolHCID 70601480HCID 70601480, 화합물

생성물 1

HCID 12401704HCID 12401704, 화합물수율 86%

실험 절차

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°.

후처리

  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

출처 및 근거

ORD 기록
ord-b4026119675d4501b228acc94bfb1628
출처 데이터셋
uspto-grants-1979_06
특허 번호
US04158663

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