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Bromine → 3-(2-Bromo-5-morpholinophenoxy)pyridin-2-amine

HRID 911893
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인쇄 미리보기

반응식

HRID 911893 반응식
[O:1]1[CH2:6][CH2:5][N:4]([C:7]2[CH:8]=[C:9]([CH:18]=[CH:19][CH:20]=2)[O:10][C:11]2[C:12]([NH2:17])=[N:13][CH:14]=[CH:15][CH:16]=2)[CH2:3][CH2:2]1.[Br:21]Br>C(O)(=O)C>[Br:21][C:18]1[CH:19]=[CH:20][C:7]([N:4]2[CH2:5][CH2:6][O:1][CH2:2][CH2:3]2)=[CH:8][C:9]=1[O:10][C:11]1[C:12]([NH2:17])=[N:13][CH:14]=[CH:15][CH:16]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 24408BromineHCID 669950653-(3-Morpholinophenoxy)pyridin-2-amine

생성물 1

HCID 669953443-(2-Bromo-5-morpholinophenoxy)pyridin-2-amine수율 77.5%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

In a 250 mL round-bottom flask, 3-(3-morpholinophenoxy)pyridin-2-amine (0.720 g, 2.654 mmol) was dissolved in 25 mL of acetic acid and Bromine (2.654 mL, 2.654 mmol) (1M in AcOH) was added slowly. After agitating for 1 hour the mixture was evaporated and the residue was distributed between dichloromethane and sodium bicarbonate solution. The organic phase was separated and evaporated. The residue was purified by column chromatography on silica gel, eluted with 1-3% methanol/dichloromethane to give the title compound (0.72 g, 77%) as white solid.

후처리

  1. customwas evaporated
  2. customThe organic phase was separated
  3. customevaporated
  4. customThe residue was purified by column chromatography on silica gel
  5. washeluted with 1-3% methanol/dichloromethane

출처 및 근거

ORD 기록
ord-b0bf5c8e94bd4df2a62a93d32f1d5877
출처 데이터셋
uspto-grants-2011_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08022223B2

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