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Isopropyl iodide → Benzonitrile, 3-methoxy-4-(1-methylethoxy)-

HRID 870523
ノート
印刷プレビュー

反応式

HRID 870523 の反応式
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[O:10][CH3:11].C(=O)([O-])[O-].[K+].[K+].[CH:18](I)([CH3:20])[CH3:19]>CC(C)=O>[CH:18]([O:1][C:2]1[CH:9]=[CH:8][C:5]([C:6]#[N:7])=[CH:4][C:3]=1[O:10][CH3:11])([CH3:20])[CH3:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 6362Isopropyl iodideHCID 11430Potassium CarbonateHCID 781354-Hydroxy-3-methoxybenzonitrile

生成物 1

HCID 2125297Benzonitrile, 3-methoxy-4-(1-methylethoxy)-

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

25 g 4-Hydroxy-3-methoxy-benzonitrile, 27.8 g potassium carbonate and 33.5 mL isopropyl iodide were placed in 250 mL acetone and heated to reflux where they were maintained for 22 h. After this time the mixture was cooled to ambient temperature and concentrated under reduced pressure. The crude product was partitioned between ethyl acetate and water and the aqueous phase was separated and extracted with additional ethyl acetate. The combined organic fractions were dried, filtered and the solvent was removed from the filtrate under reduced pressure to give the title compound which was used without further purification.

後処理

  1. temperatureheated
  2. temperatureto reflux where they
  3. temperaturewere maintained for 22 h
  4. concentrationconcentrated under reduced pressure
  5. customThe crude product was partitioned between ethyl acetate and water
  6. customthe aqueous phase was separated
  7. extractionextracted with additional ethyl acetate
  8. customThe combined organic fractions were dried
  9. filtrationfiltered
  10. customthe solvent was removed from the filtrate under reduced pressure

出典と根拠

ORDレコード
ord-e7a06437569441fda1488f5945673c62
出典データセット
uspto-grants-2015_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08969568B2

反応ノート

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