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

HRID 1741063노트

반응식

HRID 1741063 반응식
[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]

참가 물질

4

반응물 3

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

생성물 1

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

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-b21d4f72032e4fefbcae8baefd5bd2b4
출처 데이터셋
uspto-grants-1999_10
특허 번호
US05972951

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