Benzene → HCID 19096630, 화합물

HRID 486852노트

반응식

HRID 486852 반응식
[Cl:1][CH2:2][CH:3]1[O:8][C:7](=[O:9])[CH2:6][CH:5](O)[CH2:4]1.C1(C)C=CC(S(O)(=O)=O)=CC=1.C1C=CC=CC=1>C(OCC)(=O)C>[Cl:1][CH2:2][C:3]1[O:8][C:7](=[O:9])[CH2:6][CH2:5][CH:4]=1

참가 물질

5

반응물 3

HCID 241Benzene2회HCID 6101p-Toluenesulfonic acidHCID 22556038HCID 22556038, 화합물

생성물 1

HCID 19096630HCID 19096630, 화합물수율 81%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

A mixture of 50 mg (0.304 mmol) of (+)-6-chloromethyl-4-hydroxytetrahydropyran-2-one obtained in Example 3, 57.8 mg (0.304 mmol) of p-toluenesulfonic acid and 5 ml of benzene was refluxed for 30 minutes. After completion of the reaction, benzene was distilled off and distilled water were added thereto, and the solution was extracted with dichloromethane, followed by drying over anhydrous magnesium sulfate. After the solvent was distilled off, the resultant residue was subjected to column chromatography (an eluent of hexane:ethyl acetate=4:1), thereby obtaining 35.8 mg (yield 81%) of (-)-6- chloromethyldihydropyran-2-one.

후처리

  1. temperaturewas refluxed for 30 minutes
  2. distillationwas distilled off
  3. distillationdistilled water
  4. additionwere added
  5. extractionthe solution was extracted with dichloromethane
  6. dry with materialby drying over anhydrous magnesium sulfate
  7. distillationAfter the solvent was distilled off

출처 및 근거

ORD 기록
ord-d9bf080b1ce74292a2a26552e14be1bd
출처 데이터셋
uspto-grants-1994_03
특허 번호
US05292891

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