1-Iodo-3-methylbutane → HCID 21402622, 화합물

HRID 973267노트

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HRID 973267 반응식
[OH:1][C:2]1[C:7]2[C:8](=[O:17])[CH:9]=[C:10]([C:12]([O:14]CC)=[O:13])[O:11][C:6]=2[CH:5]=[CH:4][CH:3]=1.[Tl].I[CH2:20][CH2:21][CH:22]([CH3:24])[CH3:23]>C(Cl)(Cl)Cl>[CH3:23][CH:22]([CH3:24])[CH2:21][CH2:20][O:1][C:2]1[C:7]2[C:8](=[O:17])[CH:9]=[C:10]([C:12]([OH:14])=[O:13])[O:11][C:6]=2[CH:5]=[CH:4][CH:3]=1

참가 물질

5

반응물 3

HCID 109241-Iodo-3-methylbutaneHCID 2801504ethyl 5-hydroxy-4-oxo-4H-chromene-2-carboxylateHCID 5359464Thallium

생성물 1

HCID 21402622HCID 21402622, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

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온도
100 °C

실험 절차

A stirred mixture of 21.67 parts of ethyl 5-hydroxy-4-oxo-4H-1-benzopyran-2-carboxylate, thallium salt and 99 parts of 1-iodo-3-methylbutane was refluxed for one hour. After cooling, chloroform was added to the reaction mixture and the insoluble thallium salts were removed by filtration. The chloroform filtrate was washed with cold N sodium hydroxide solution, then washed with water and the volatile components were removed by evaporation. Sodiumbicarbonte soluton was added to the oily residue obtained and the mixture was stirred at 100° C for 2 hours. After cooling, the solution ws extracted with chloroform and the aqueous layer was separated. This aqueous extract was acidified with 2H hydrochloric acid and the solid which precipitated was collected by filtration, washed with water and dried to give 6.16 parts of 5-(3-methyl-n-butoxy)-4-oxo-4H-1-benzopyran-2-carboxylic acid, m.p. 181°-183° C (after crystallistion from ethyl acetate/light petroleum.

후처리

  1. temperaturewas refluxed for one hour
  2. temperatureAfter cooling
  3. customthe insoluble thallium salts were removed by filtration
  4. washThe chloroform filtrate was washed with cold N sodium hydroxide solution
  5. washwashed with water
  6. customthe volatile components were removed by evaporation
  7. additionSodiumbicarbonte soluton was added to the oily residue
  8. customobtained
  9. temperatureAfter cooling
  10. extractionthe solution ws extracted with chloroform
  11. customthe aqueous layer was separated
  12. extractionThis aqueous extract
  13. customthe solid which precipitated
  14. filtrationwas collected by filtration
  15. washwashed with water
  16. customdried

출처 및 근거

ORD 기록
ord-a692ffbb1cbd455a95eb28441e465954
출처 데이터셋
uspto-grants-1977_10
특허 번호
US04055654

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