Sodium Iodide → Benzonitrile, 4-[(5-iodopentyl)oxy]-

HRID 732246

반응식

HRID 732246 반응식
Cl[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][O:7][C:8]1[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[CH:10][CH:9]=1.CC(=O)CC.[I-:21].[Na+]>C(OC(=O)C)C>[I:21][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][O:7][C:8]1[CH:15]=[CH:14][C:11]([C:12]#[N:13])=[CH:10][CH:9]=1

참가 물질

5

반응물 3

HCID 5238Sodium IodideHCID 6569Methyl Ethyl KetoneHCID 193815104-((5-Chloropentyl)oxy)benzonitrile

생성물 1

HCID 16202445Benzonitrile, 4-[(5-iodopentyl)oxy]-수율 99%

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

While 50 g of 4-(5-chloro-pentoxy)-benzonitrile (8) prepared in Example 5 were added to 500 ml of 2-butanone and stirred, 167 g of sodium iodide were added. Subsequently, the reaction temperature was gradually increased and stirring was continued at 70-80° C. for 6 hr. After the reaction was completed, the reaction temperature was decreased to room temperature, and the resultant reaction mixture was added with 1 L of ethylacetate, and then washed with water and brine. The ethylacetate layer was dried over anhydrous magnesium sulfate, and then concentrated under reduced pressure. The residual solution was crystallized with methylalcohol, thus obtaining 69.7 g (yield: 99%) of a title compound as a white solid.

후처리

  1. temperatureSubsequently, the reaction temperature was gradually increased
  2. stirringstirring
  3. customwas decreased to room temperature
  4. customthe resultant reaction mixture
  5. washwashed with water and brine
  6. dry with materialThe ethylacetate layer was dried over anhydrous magnesium sulfate
  7. concentrationconcentrated under reduced pressure
  8. customThe residual solution was crystallized with methylalcohol

출처 및 근거

ORD 기록
ord-e4f7c9701fa94bc2b4963889c6315dde
출처 데이터셋
uspto-grants-2009_09
특허 번호
US07585979B2

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