Acetic Acid → 5-Ethoxy-3-(3-iodophenyl)-1H-1,2,4-triazole

HRID 1372475ノート

反応式

HRID 1372475 の反応式
[NH2:1][N:2]1[CH2:6][N:5]=[C:4]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([I:13])[CH:8]=2)O1.[OH-].[K+].[C:16](O)(=[O:18])[CH3:17]>C(O)C>[CH2:16]([O:18][C:6]1[NH:2][N:1]=[C:4]([C:7]2[CH:12]=[CH:11][CH:10]=[C:9]([I:13])[CH:8]=2)[N:5]=1)[CH3:17]

参加物

5

反応物 3

HCID 176Acetic AcidHCID 14797Potassium HydroxideHCID 69373404HCID 69373404、化合物

生成物 1

HCID 1784673965-Ethoxy-3-(3-iodophenyl)-1H-1,2,4-triazole

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

The product (1.00 g, 3.48 mmol) from Step A was added to a solution of potassium hydroxide (1.0 g) in 30 mL of absolute ethanol. The mixture was warmed to reflux and, after 5 h, cooled to room temperature. The solution was then acidified with glacial acetic acid, and concentrated under reduced pressure. The product was extracted into ethyl acetate, and the combined ethyl acetate extracts were washed sequentially with water and saturated aqueous brine, dried (magnesium sulfate) and concentrated to give the crude product as an orange semisolid. Purification by flash chromatography (silica gel, 15% ethyl acetate-hexanes) afforded the product as an off-white, sticky foam. LC/MS 316.0 (M+1).

後処理

  1. temperatureThe mixture was warmed
  2. temperatureto reflux and, after 5 h
  3. concentrationconcentrated under reduced pressure
  4. extractionThe product was extracted into ethyl acetate
  5. washthe combined ethyl acetate extracts were washed sequentially with water and saturated aqueous brine
  6. dry with materialdried (magnesium sulfate)
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-e78a9204f96c43e3ae9dbd94741185ab
出典データセット
uspto-grants-2007_01
特許番号
US07157490B2

反応ノート

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