Water → HCID 18466625, 화합물

HRID 2229306노트

반응식

HRID 2229306 반응식
[Br:1][C:2]1[CH:3]=[C:4]([C:9](Cl)=[O:10])[C:5]([Cl:8])=[N:6][CH:7]=1.[NH2:12][C:13]1[C:14]([NH:20][CH2:21][CH3:22])=[N:15][C:16]([Cl:19])=[CH:17][CH:18]=1.C([O-])(O)=O.[Na+].O>CC#N>[Br:1][C:2]1[CH:3]=[C:4]([C:9]([NH:12][C:13]2[C:14]([NH:20][CH2:21][CH3:22])=[N:15][C:16]([Cl:19])=[CH:17][CH:18]=2)=[O:10])[C:5]([Cl:8])=[N:6][CH:7]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 516892Sodium BicarbonateHCID 10797271HCID 10797271, 화합물HCID 126772955-Bromo-2-chloro-3-pyridinecarbonyl chloride

생성물 1

HCID 18466625HCID 18466625, 화합물수율 75.1%

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

A solution of 5-bromo-2-chloro-3-pyridinecarbonyl chloride (30.0 g, 97.0 mmol) in MeCN (100 mL) was added via cannula to a solution of 3-amino-6-chloro-2-(ethylamino)pyridine (16.6 g, 97.0 mmol) in MeCN (180 mL) containing solid NaHCO3 (14.2 g, 169 mmol) at room temperature. The mixture was stirred at room temperature for 1 h. Water (200 mL) was added and the mixture was stirred for 10 min. The resulting suspension was filtered. The solid was washed with Et2O (50 mL) and concentrated from pyridine solution (3×50 mL) to give the title compound (28.4 g, 75% yield).

후처리

  1. stirringthe mixture was stirred for 10 min
  2. filtrationThe resulting suspension was filtered
  3. washThe solid was washed with Et2O (50 mL)
  4. concentrationconcentrated from pyridine solution (3×50 mL)

출처 및 근거

ORD 기록
ord-1f98b504cb8a4793ab3cab7d384dd18a
출처 데이터셋
uspto-grants-2002_07
특허 번호
US06420359B1

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