Potassium Cyanide → HCID 19092790、化合物

HRID 487682ノート

反応式

HRID 487682 の反応式
[C:1]([C:5]1[N:6]=[C:7]([C:10]2[O:11][C:12]3[CH:18]=[CH:17][C:16]([O:19][CH2:20][C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=4[CH2:27]Cl)=[CH:15][C:13]=3[CH:14]=2)[S:8][CH:9]=1)([CH3:4])([CH3:3])[CH3:2].[C-:29]#[N:30].[K+]>CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)C.[Cl-].C1(C)C=CC=CC=1.O>[C:1]([C:5]1[N:6]=[C:7]([C:10]2[O:11][C:12]3[CH:18]=[CH:17][C:16]([O:19][CH2:20][C:21]4[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=4[CH2:27][C:29]#[N:30])=[CH:15][C:13]=3[CH:14]=2)[S:8][CH:9]=1)([CH3:4])([CH3:3])[CH3:2]

参加物

6

反応物 2

HCID 9032Potassium CyanideHCID 190928204-Tert-butyl-2-[5-(2-chloromethylphenylmethoxy)benzofuran-2-yl]thiazole

生成物 1

HCID 19092790HCID 19092790、化合物収率 85.7%

試薬・触媒・溶媒 3

HCID 21218Trioctylmethylammonium chloride触媒HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

A mixture of 4-tert-butyl-2-[5-(2-chloromethylphenylmethoxy)benzofuran-2-yl]thiazole (0.8 g), potassium cyanide (0.25 g) and Adogen 464 ((Aldrich phase transfer) one drop) in a mixture of toluene (8 ml) and water (8 ml) was stirred under reflux for 4 hours. After being cooled, the organic layer was separated, washed with brine, dried over magnesium sulfate and concentrated in reduced pressure. The resulting residue was subjected to column chromatography on silica gel and eluted with toluene. The fractions containing object compound were combined and concentrated under reduced pressure to give an oil of 4-tert-butyl-2-[5-(2-cyanomethylphenylmethoxy)benzofuran-2-yl]thiazole (0.67 g).

後処理

  1. temperatureunder reflux for 4 hours
  2. temperatureAfter being cooled
  3. customthe organic layer was separated
  4. washwashed with brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated in reduced pressure
  7. washeluted with toluene
  8. additionThe fractions containing object compound
  9. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-3828fde968884821bfc0bee25c42bbb0
出典データセット
uspto-grants-1994_03
特許番号
US05296495

反応ノート

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