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Cyclopropylamine → HCID 18466610, 화합물

HRID 2229330
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인쇄 미리보기

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HRID 2229330 반응식
[Br:1][C:2]1[CH:3]=[C:4]([C:9]([NH:11][C:12]2[C:13]([Cl:20])=[N:14][C:15]([Cl:19])=[CH:16][C:17]=2[CH3:18])=[O:10])[C:5](Cl)=[N:6][CH:7]=1.[CH:21]1([NH2:24])[CH2:23][CH2:22]1>O>[Br:1][C:2]1[CH:3]=[C:4]([C:9]([NH:11][C:12]2[C:13]([Cl:20])=[N:14][C:15]([Cl:19])=[CH:16][C:17]=2[CH3:18])=[O:10])[C:5]([NH:24][CH:21]2[CH2:23][CH2:22]2)=[N:6][CH:7]=1
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참가 물질

4

반응물 2

HCID 69828CyclopropylamineHCID 18466614HCID 18466614, 화합물

생성물 1

HCID 18466610HCID 18466610, 화합물수율 75%

시약·촉매·용매 1

HCID 962Water용매

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온도
0 °C

실험 절차

A solution of 5-bromo-2-chloro-N-(2,6-dichloro-4-methyl-3-pyridinyl)-3-pyridinecarboxamide (3.00 g, 7.61 mmol) and cyclopropylamine (2.11 mL, 30.5 mmol) in xylenes was heated in a sealed tube at 120° C. for 24 h. The reaction was cooled to 0° C., diluted with water and extracted with EtOAc (2×). The combined organic extracts were dried (MgSO4), filtered and concentrated under reduced pressure. The resulting residue was purified by trituration (Et2O:hexane, 3:1) to give the title compound (2.35 g, 75% yield) as a pale yellow solid.

후처리

  1. extractionextracted with EtOAc (2×)
  2. dry with materialThe combined organic extracts were dried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting residue was purified by trituration (Et2O:hexane, 3:1)

출처 및 근거

ORD 기록
ord-3d8dbda2bf32418b8fafdd878830094b
출처 데이터셋
uspto-grants-2002_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06420359B1

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