Bromine → HCID 22625622、化合物

HRID 1600552ノート

反応式

HRID 1600552 の反応式
[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]

参加物

5

反応物 3

HCID 24408BromineHCID 516892Sodium BicarbonateHCID 22625614HCID 22625614、化合物

生成物 1

HCID 22625622HCID 22625622、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

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.).

後処理

  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)

出典と根拠

ORDレコード
ord-d828f045807c462e83aa32e43b7cf221
出典データセット
uspto-grants-1999_11
特許番号
US05977028

反応ノート

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