Triethylamine → 2-Thiazolamine, 4-(4-methoxyphenyl)-5-(3-pyridinyl)-

HRID 1062616

반응식

HRID 1062616 반응식
[NH2:1][C:2]([NH2:4])=[S:3].Br.Br[CH:7]([C:18]1[CH:19]=[N:20][CH:21]=[CH:22][CH:23]=1)[C:8]([C:10]1[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[CH:12][CH:11]=1)=O.C(N(CC)CC)C>C(#N)C>[CH3:17][O:16][C:13]1[CH:12]=[CH:11][C:10]([C:8]2[N:1]=[C:2]([NH2:4])[S:3][C:7]=2[C:18]2[CH:19]=[N:20][CH:21]=[CH:22][CH:23]=2)=[CH:15][CH:14]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 2723790ThioureaHCID 114633362-Bromo-1-(4-methoxyphenyl)-2-(3-pyridyl)ethanone hydrobromide

생성물 1

HCID 30248942-Thiazolamine, 4-(4-methoxyphenyl)-5-(3-pyridinyl)-수율 90%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

To a suspension of thiourea (0.52 g) in acetonitrile (40 mL) was added 2-bromo-1-(4-methoxyphenyl)-2-(3-pyridyl)ethanone hydrobromide (2.5 g) and triethylamine (0.95 mL) was slowly added dropwise with stirring. After completion of dropwise addition, the mixture was stirred at a refluxing temperature for 3 h, and after allowing to cool, the precipitated crystals were collected by filtration. The crystals were washed successively with saturated sodium hydrogencarbonate solution, water, ethanol and ethyl ether and dried. The obtained crude crystals were recrystallized from tetrahydrofuran to give the title compound (1.5 g, yield 90%).

후처리

  1. additionwas slowly added dropwise
  2. additionAfter completion of dropwise addition
  3. stirringthe mixture was stirred at a refluxing temperature for 3 h
  4. temperatureto cool
  5. filtrationthe precipitated crystals were collected by filtration
  6. washThe crystals were washed successively with saturated sodium hydrogencarbonate solution, water, ethanol and ethyl ether
  7. customdried
  8. customThe obtained crude crystals
  9. customwere recrystallized from tetrahydrofuran

출처 및 근거

ORD 기록
ord-e133ce62de6947f8bb67d304a85fa7b6
출처 데이터셋
uspto-grants-2005_11
특허 번호
US06962933B1

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