Water → 3-ethoxy-1,5-bis(4-methoxyphenyl)-1H-1,2,4-triazole

HRID 584739ノート

反応式

HRID 584739 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([N:9]2[C:13]([C:14]3[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=3)=[N:12][C:11]([OH:22])=[N:10]2)=[CH:5][CH:4]=1.C(=O)([O-])[O-].[K+].[K+].I[CH2:30][CH3:31].O>CN(C)C=O.C(OCC)(=O)C.O1CCCC1>[CH2:30]([O:22][C:11]1[N:12]=[C:13]([C:14]2[CH:19]=[CH:18][C:17]([O:20][CH3:21])=[CH:16][CH:15]=2)[N:9]([C:6]2[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:8][CH:7]=2)[N:10]=1)[CH3:31]

参加物

7

反応物 4

HCID 962WaterHCID 6340IodoethaneHCID 11430Potassium CarbonateHCID 1784890151,5-bis(4-methoxyphenyl)-1H-1,2,4-triazol-3-ol

生成物 1

HCID 102681963-ethoxy-1,5-bis(4-methoxyphenyl)-1H-1,2,4-triazole収率 43.6%

試薬・触媒・溶媒 2

HCID 6228Dimethylformamide溶媒HCID 21939870Tetrahydrofuran ethyl acetate溶媒

実験手順

A mixture of 1,5-bis(4-methoxyphenyl)-1H-1,2,4-triazol-3-ol (0.3 g, 1.01 mmol), potassium carbonate (418 mg, 3.01 mmol), and iodoethane (0.406 mL, 5.05 mmol) in dimethylformamide (3 mL) was stirred for 3 days. Water and ethyl acetate-tetrahydrofuran (9:1) were poured into the mixture and the organic layer was separated, washed with brine-water (1:1) and brine, and dried over magnesium sulfate. The solvent was removed under reduced pressure. The residue was purified by column chromatography to give 3-ethoxy-1,5-bis(4-methoxyphenyl)-1H-1,2,4-triazole (143 mg, 43.6% yield).

後処理

  1. customthe organic layer was separated
  2. washwashed with brine-water (1:1) and brine
  3. dry with materialdried over magnesium sulfate
  4. customThe solvent was removed under reduced pressure
  5. customThe residue was purified by column chromatography

出典と根拠

ORDレコード
ord-773e96a0272e4f7f91316d00bb8578c8
出典データセット
uspto-grants-2005_08
特許番号
US06927230B2

反応ノート

読み込み中…