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Water → HCID 178489961、化合物

HRID 620826
ノート
印刷プレビュー

反応式

HRID 620826 の反応式
O[N:2]1[C:6]([C:7]2[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=2)=[C:5]([CH3:13])[N:4]=[C:3]1[C:14]1[CH:19]=[CH:18][C:17]([CH3:20])=[CH:16][C:15]=1[O:21][CH3:22].P(Cl)(Cl)Cl.O.C(=O)(O)[O-].[Na+]>CN(C)C=O>[CH3:22][O:21][C:15]1[CH:16]=[C:17]([CH3:20])[CH:18]=[CH:19][C:14]=1[C:3]1[NH:2][C:6]([C:7]2[CH:8]=[N:9][CH:10]=[CH:11][CH:12]=2)=[C:5]([CH3:13])[N:4]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 24387Phosphorus trichlorideHCID 516892Sodium BicarbonateHCID 100858711-Hydroxy-2-(2-methoxy-4-methylphenyl)-4-methyl-5-(3-pyridyl)imidazole

生成物 1

HCID 178489961HCID 178489961、化合物収率 61.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide
溶媒

実験手順

To a solution of 1-hydroxy-2-(2-methoxy-4-methylphenyl)-4-methyl-5-(3-pyridyl)imidazole (1.40 g) in N,N-dimethylformamide (28 ml), was added phosphorus trichloride (0.83 ml), and the mixture was stirred for 2 hours at ambient temperature. Then, the solution was poured into water (150 ml), and stirred for an hour at ambient temperature. After neutrallized with aqueous sodium bicarbonate, resulting precipitates were collected by filtration. The precipitates were dried, dissolved in chloroform, and chromatographed on silica gel eluting with a mixture of chloroform and methanol. The fractions were collected, evaporated and triturated in diisopropyl ether to give 2-(2-methoxy-4-methylphenyl)-4-methyl-5-(3-pyridyl)imidazole (0.82 g)

後処理

  1. stirringstirred for an hour at ambient temperature
  2. customresulting
  3. customprecipitates
  4. filtrationwere collected by filtration
  5. customThe precipitates were dried
  6. dissolutiondissolved in chloroform
  7. customchromatographed on silica gel eluting with a mixture of chloroform and methanol
  8. customThe fractions were collected
  9. customevaporated
  10. customtriturated in diisopropyl ether

出典と根拠

ORDレコード
ord-fea94de4fd114f25872f76e505de23f5
出典データセット
uspto-grants-1989_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04822805

反応ノート

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