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

HRID 732246

反応式

HRID 732246 の反応式
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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-e4f7c9701fa94bc2b4963889c6315dde
出典データセット
uspto-grants-2009_09
特許番号
US07585979B2

関連ノート

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