Water → (5-Bromo-6-chloro-pyridin-2-yl)-(4-chloro-benzyl)-amine

HRID 1754728노트

반응식

HRID 1754728 반응식
[Cl:1][C:2]1[CH:16]=[CH:15][C:5]([CH2:6][NH:7][C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([Cl:14])[N:9]=2)=[CH:4][CH:3]=1.[Br:17]N1C(=O)CCC1=O.O>C(#N)C>[Br:17][C:11]1[CH:12]=[CH:13][C:8]([NH:7][CH2:6][C:5]2[CH:15]=[CH:16][C:2]([Cl:1])=[CH:3][CH:4]=2)=[N:9][C:10]=1[Cl:14]

참가 물질

5

반응물 3

HCID 962WaterHCID 67184N-bromobutanimideHCID 57619237(4-Chloro-benzyl)-(6-chloro-pyridin-2-yl)-amine

생성물 1

HCID 57619309(5-Bromo-6-chloro-pyridin-2-yl)-(4-chloro-benzyl)-amine

시약·촉매·용매 1

HCID 6342Acetonitrile용매2회

실험 절차

To (4-chloro-benzyl)-(6-chloro-pyridin-2-yl)-amine (538, 4.00 g, 0.0158 mol) in acetonitrile (66.7 mL, 1.28 mol) under an atmosphere of nitrogen, N-bromosuccinimide (2.81 g, 0.0158 mol) in acetonitrile (20 mL) was added slowly. The reaction was stirred at room temperature overnight, then poured into water and extracted with ethyl acetate. The organic layer was dried over sodium sulfate, concentrated and crystallized with ethyl acetate in hexane to give a white solid (539, 2.60 g, 95.3%).

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic layer was dried over sodium sulfate
  3. concentrationconcentrated
  4. customcrystallized with ethyl acetate in hexane
  5. customto give a white solid (539, 2.60 g, 95.3%)

출처 및 근거

ORD 기록
ord-15f917479d7a4133b04098b042ae33c6
출처 데이터셋
uspto-grants-2015_10
특허 번호
US09169250B2

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