Triethylamine → 3-(4-Bromo-3-methylphenyl)-5-methyl-1,2,4-triazole

HRID 1741063ノート

反応式

HRID 1741063 の反応式
[Br:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]([NH:8][NH2:9])=O)=[CH:4][C:3]=1[CH3:12].Cl.[C:14](=[NH:19])(OCC)[CH3:15].C(N(CC)CC)C>>[Br:1][C:2]1[CH:11]=[CH:10][C:5]([C:6]2[N:19]=[C:14]([CH3:15])[NH:9][N:8]=2)=[CH:4][C:3]=1[CH3:12]

参加物

4

反応物 3

HCID 8471TriethylamineHCID 2724290Ethanimidic acid, ethyl ester, hydrochloride (1:1)HCID 39058874-Bromo-3-methylbenzohydrazide

生成物 1

HCID 218338103-(4-Bromo-3-methylphenyl)-5-methyl-1,2,4-triazole収率 59.5%

実験手順

4-Bromo-3-methylbenzoic hydrazide (D30, 3.06 g, 13 mmol), ethyl acetimidate hydrochloride (2.48 g, 20 mmol) and triethylamine (5.6 ml, 40 mmol) were stirred at reflux under Ar for 24 h, and then evaporated to dryness. The residue was chromatographed on silica gel, eluting with dichloromethane/ethanol/ammonia (300:8:1). This gave the title compound (1.95 g, 58%) as a white solid.

後処理

  1. temperatureat reflux under Ar for 24 h
  2. customevaporated to dryness
  3. customThe residue was chromatographed on silica gel
  4. washeluting with dichloromethane/ethanol/ammonia (300:8:1)

出典と根拠

ORDレコード
ord-b21d4f72032e4fefbcae8baefd5bd2b4
出典データセット
uspto-grants-1999_10
特許番号
US05972951

反応ノート

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