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

HRID 1372475노트

반응식

HRID 1372475 반응식
[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]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 14797Potassium HydroxideHCID 69373404HCID 69373404, 화합물

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e78a9204f96c43e3ae9dbd94741185ab
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07157490B2

반응 노트

불러오는 중…