Bromine → HCID 22625622, 화합물

HRID 1600552노트

반응식

HRID 1600552 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[CH:4][C:3]=1[C:9]1[N:10]=[C:11]2[CH2:16][CH2:15][CH2:14][CH2:13][N:12]2[CH:17]=1.[Br:18]Br.C(=O)(O)[O-].[Na+]>C(Cl)Cl>[Br:18][C:17]1[N:12]2[CH2:13][CH2:14][CH2:15][CH2:16][C:11]2=[N:10][C:9]=1[C:3]1[CH:4]=[CH:5][C:6]([Cl:8])=[CH:7][C:2]=1[Cl:1]

참가 물질

5

반응물 3

HCID 24408BromineHCID 516892Sodium BicarbonateHCID 22625614HCID 22625614, 화합물

생성물 1

HCID 22625622HCID 22625622, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매3회

실험 절차

To 0.8 g (3.0 mmol) of the above 2-(2,4-dichlorophenyl)-5,6,7,8-tetrahydroimidazo[1,2-a]pyridine stirring in 50 ml of methylene chloride at room temperature, 0.5 g (3.1 mmol) of bromine in 5 ml of methylene chloride was added dropwise. The solution was stirred for 2 h. Another 20 ml of methylene chloride and excess saturated aqueous sodium bicarbonate were added. After sufficient mixing, the methylene chloride layer was separated, washed with water and brine, and dried over magnesium sulfate. Evaporating the solvent in vacuo gave a yellow solid residue which was purified by silica gel column chromatography (5:1 followed by 3:1 followed in turn by 1:1 hexane/ethyl acetate) to yield a 0.55 g sample of the title compound (m.p. 112-113° C.).

후처리

  1. customAfter sufficient mixing, the methylene chloride layer was separated
  2. washwashed with water and brine
  3. dry with materialdried over magnesium sulfate
  4. customEvaporating the solvent in vacuo
  5. customgave a yellow solid residue which
  6. customwas purified by silica gel column chromatography (5:1 followed by 3:1 followed in turn by 1:1 hexane/ethyl acetate)

출처 및 근거

ORD 기록
ord-d828f045807c462e83aa32e43b7cf221
출처 데이터셋
uspto-grants-1999_11
특허 번호
US05977028

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