Triethylamine → 1-(7-Bromo-3-nitroquinolin-4-ylamino)-2-methylpropan-2-ol

HRID 9378

반응식

HRID 9378 반응식
C(N(CC)CC)C.[Br:8][C:9]1[CH:18]=[C:17]2[C:12]([C:13](Cl)=[C:14]([N+:19]([O-:21])=[O:20])[CH:15]=[N:16]2)=[CH:11][CH:10]=1.[NH2:23][CH2:24][C:25]([CH3:28])([OH:27])[CH3:26]>ClCCl>[Br:8][C:9]1[CH:18]=[C:17]2[C:12]([C:13]([NH:23][CH2:24][C:25]([CH3:28])([OH:27])[CH3:26])=[C:14]([N+:19]([O-:21])=[O:20])[CH:15]=[N:16]2)=[CH:11][CH:10]=1

참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 951022-Propanol, 1-amino-2-methyl-HCID 219843617-Bromo-4-chloro-3-nitroquinoline

생성물 1

HCID 219844361-(7-Bromo-3-nitroquinolin-4-ylamino)-2-methylpropan-2-ol수율 78.5%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

반응 조건

온도
0 °C

실험 절차

Triethylamine (17.35 mL, 124 mmol) was added to a solution of 7-bromo-4-chloro-3-nitroquinoline (29.84 g, 104 mmol) in dichloromethane (253 mL), and the reaction was cooled to 0° C. 1-Amino-2-methylpropan-2-ol (10.17 g, 114 mmol) was added dropwise, and then the reaction was allowed to warm to ambient temperature and stirred overnight. A precipitate formed and was isolated by filtration and washed with water. The crude solid was recrystallized from a mixture of isopropanol and acetonitrile to provide 27.78 g of 1-(7-bromo-3-nitroquinolin-4-ylamino)-2-methylpropan-2-ol as a solid.

후처리

  1. temperatureto warm to ambient temperature
  2. customA precipitate formed
  3. customwas isolated by filtration
  4. washwashed with water
  5. customThe crude solid was recrystallized from a mixture of isopropanol and acetonitrile

출처 및 근거

ORD 기록
ord-264de42745e6441b818c0fd73a192dd5
출처 데이터셋
uspto-grants-2006_08
특허 번호
US07091214B2

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