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Calcium Chloride → Benzenamine,4-[(imidazo[1,2-a]pyridin-3-ylmethyl)thio]-

HRID 856662
ノート
印刷プレビュー

反応式

HRID 856662 の反応式
[N+:1]([C:4]1[CH:9]=[CH:8][C:7]([S:10][CH2:11][C:12]2[N:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]3=[N:14][CH:13]=2)=[CH:6][CH:5]=1)([O-])=O.[Cl-].[Ca+2].[Cl-]>C(O)C>[NH2:1][C:4]1[CH:9]=[CH:8][C:7]([S:10][CH2:11][C:12]2[N:16]3[CH:17]=[CH:18][CH:19]=[CH:20][C:15]3=[N:14][CH:13]=2)=[CH:6][CH:5]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 5284359Calcium ChlorideHCID 229383933-(4-Nitrophenylthiomethyl)imidazo[1,2-a]pyridine

生成物 1

HCID 22938675Benzenamine,4-[(imidazo[1,2-a]pyridin-3-ylmethyl)thio]-収率 84.2%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A mixture of 3-(4-nitrophenylthiomethyl)imidazo[1,2-a]pyridine (1.5 g), reduced iron (1.47 g) and calcium chloride (0.29 g) in 15% hydrous ethanol (45 ml) was heated to reflux for 5 hours. After cooling to room temperature, and the precipitates were removed by filtration. After concentrating the filtrate, water was added to the mixture and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated brine, dried over magnesium sulfate and concentrated under reduced pressure. The precipitated crystals were collected by filtration. The crystals were washed with diisopropylether, to give 3-(4-aminophenylthiomethyl)imidazo[1,2-a]pyridine (1.13 g) as pale yellow crystals.

後処理

  1. temperaturewas heated
  2. temperatureto reflux for 5 hours
  3. customthe precipitates were removed by filtration
  4. concentrationAfter concentrating the filtrate, water
  5. additionwas added to the mixture
  6. extractionthe mixture was extracted with ethyl acetate
  7. washThe organic layer was washed with saturated brine
  8. dry with materialdried over magnesium sulfate
  9. concentrationconcentrated under reduced pressure
  10. filtrationThe precipitated crystals were collected by filtration
  11. washThe crystals were washed with diisopropylether

出典と根拠

ORDレコード
ord-72b251f80b084310822916fe9048e6c0
出典データセット
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07262185B2

反応ノート

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