Potassium Carbonate → 92642-95-0

HRID 1660493노트

반응식

HRID 1660493 반응식
Br[CH:2]([CH2:8]Br)[C:3]([O:5]CC)=[O:4].C(=O)([O-])[O-].[K+].[K+].[SH:16][C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=1[OH:23]>CC(C)=O.C(Cl)Cl>[O:23]1[C:18]2[CH:19]=[CH:20][CH:21]=[CH:22][C:17]=2[S:16][CH2:8][CH:2]1[C:3]([OH:5])=[O:4]

참가 물질

6

반응물 3

HCID 11430Potassium Carbonate2회HCID 70718Phenol, o-mercapto-(6CI,7CI,8CI)HCID 97945Ethyl 2,3-dibromopropionate

생성물 1

HCID 1340891892642-95-0

시약·촉매·용매 2

HCID 180Acetone용매2회HCID 6344Dichloromethane용매

실험 절차

To a stirred mixture of 41.6 g of ethyl 2,3-dibromopropionate, 400 ml of dry acetone and 11.1 g of potassium carbonate, there was added dropwise at 27° C. a solution of 19.5 g of o-mercaptophenol in 75 ml of acetone. After the addition was complete, the reaction mixture was stirred at room temperature for 10 minutes and an additional 50.9 g of potassium carbonate was added. The reaction mixture then was refluxed for 2 hours, and allowed to stand overnight at room temperature. The mixture was filtered and the solid was washed with acetone, the washings being added to the filtrate. The acetone was stripped to leave a liquid, which was taken up in methylene chloride. The resulting solution was washed with water and dried (MgSO4), and the solvent was stripped. The resulting liquid was dry column chromatographed through silica gel, using a 4:16:80 by volume mixture of tetrahydrofuran, ethyl acetate and hexane (Solvent No. 2) as eluent, to give the ethyl ester of 2,3-dihydro-1,4-benzoxathiin-2-carboxylic acid (1A), as a light yellow liquid, boiling point not determined.

후처리

  1. additionAfter the addition
  2. temperatureThe reaction mixture then was refluxed for 2 hours
  3. waitto stand overnight at room temperature
  4. filtrationThe mixture was filtered
  5. washthe solid was washed with acetone
  6. additionthe washings being added to the filtrate
  7. customto leave a liquid, which
  8. washThe resulting solution was washed with water
  9. dry with materialdried (MgSO4)
  10. customThe resulting liquid was dry column
  11. customchromatographed through silica gel
  12. additionby volume mixture of tetrahydrofuran, ethyl acetate and hexane (Solvent No. 2) as eluent

출처 및 근거

ORD 기록
ord-e09ce0a7b8094c7582bb5750a909a707
출처 데이터셋
uspto-grants-1981_12
특허 번호
US04308276

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