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Isopropanol → 2-Amino-3-bromo-4-(4-amino-3-chlorophenoxy)pyridine

HRID 387823
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반응식

HRID 387823 반응식
[NH2:1][C:2]1[CH:7]=[C:6]([O:8][C:9]2[CH:14]=[CH:13][C:12]([NH2:15])=[C:11]([Cl:16])[CH:10]=2)[CH:5]=[CH:4][N:3]=1.[Br:17]N1C(=O)CCC1=O.C(O)(C)C>O>[NH2:1][C:2]1[C:7]([Br:17])=[C:6]([O:8][C:9]2[CH:14]=[CH:13][C:12]([NH2:15])=[C:11]([Cl:16])[CH:10]=2)[CH:5]=[CH:4][N:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 3776IsopropanolHCID 67184N-bromobutanimideHCID 229367984-(4-Amino-3-chlorophenoxy)pyridin-2-ylamine

생성물 1

HCID 229362552-Amino-3-bromo-4-(4-amino-3-chlorophenoxy)pyridine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

2-Amino-4-(4-amino-3-chlorophenoxy)pyridine (1.0 g), N-bromosuccinimide (0.78 g) and isopropanol (10 ml) were stirred for 15 minutes under reflux. The mixture was returned to room temperature, water was added, and extraction was performed with ethyl acetate. Silica gel was added to the extract solution and the solvent was distilled off under reduced pressure. The silica gel was charged into a dry column packed with silica gel, and purification was performed by column chromatography (hexane:ethyl acetate=2:1, followed by 1:1, ethyl acetate) to obtain 400 mg of the target substance as a brown oil.

후처리

  1. temperatureunder reflux
  2. customwas returned to room temperature
  3. extractionextraction
  4. additionSilica gel was added to the extract solution
  5. distillationthe solvent was distilled off under reduced pressure
  6. additionThe silica gel was charged into a dry column
  7. custompacked with silica gel, and purification
  8. customto obtain 400 mg of the target substance as a brown oil

출처 및 근거

ORD 기록
ord-85e6938aa7914932ad6d6ab47596493b
출처 데이터셋
uspto-grants-2013_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08372981B2

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