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Potassium Iodide → 3-(4-Chlorophenyl)-5-iodo-5-methyl-oxazolidine-2,4-dione

HRID 26467
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HRID 26467 반응식
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12](=[O:13])[C:11](Br)([CH3:14])[O:10][C:9]2=[O:16])=[CH:4][CH:3]=1.[I-:17].[K+]>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1.O>[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:12](=[O:13])[C:11]([I:17])([CH3:14])[O:10][C:9]2=[O:16])=[CH:4][CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 4875Potassium IodideHCID 213237073-(4-Chlorophenyl)-5-bromo-5-methyl-oxazolidine-2,4-dione

생성물 1

HCID 213237083-(4-Chlorophenyl)-5-iodo-5-methyl-oxazolidine-2,4-dione

시약·촉매·용매 2

HCID 66133Benzyl triethylammonium chloride촉매HCID 962Water용매

실험 절차

6.1 g (0.02 mole) of the 3-(4-chlorophenyl)-5-bromo-5-methyl-oxazolidine-2,4-dione, produced in a manner analogous to that described in Example 1, and 33.2 g (0.2 mole) of potassium iodide are placed, together with a spatula tip of benzyltriethylammonium chloride, in 50 ml of water, and the mixture is stirred at 50° for 7 days. It is then cooled to room temperature, and the solid product is filtered off with suction. After washing with water, the crude product is taken up in methylene chloride, and extracted once with water. The organic phase is then dried over sodium sulphate, filtered, and concentrated in a vacuum evaporator. The substance remaining behind is digested with a small amount of ether/petroleum ether, then filtered off with suction and dried. There is obtained a yield of 3.3 g of substance having a melting point of 132°-142°.

후처리

  1. filtrationthe solid product is filtered off with suction
  2. washAfter washing with water
  3. extractionextracted once with water
  4. dry with materialThe organic phase is then dried over sodium sulphate
  5. filtrationfiltered
  6. concentrationconcentrated in a vacuum evaporator
  7. filtrationfiltered off with suction
  8. customdried
  9. customThere is obtained a yield of 3.3 g of substance

출처 및 근거

ORD 기록
ord-ea6bdc68b4f04cdbad0f3478d9dc9e09
출처 데이터셋
uspto-grants-1979_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04150144

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