Imidazole → HCID 14419323、化合物

HRID 1808670ノート

反応式

HRID 1808670 の反応式
[NH:1]1[CH:5]=[CH:4][N:3]=[CH:2]1.[H-].[Na+].I[CH2:9][CH2:10][CH2:11][Si:12]([O:17][CH3:18])([O:15][CH3:16])[O:13][CH3:14].ClCCl>O1CCCC1>[CH3:14][O:13][Si:12]([CH2:11][CH2:10][CH2:9][C:2]1[NH:1][CH:5]=[CH:4][N:3]=1)([O:17][CH3:18])[O:15][CH3:16]

参加物

6

反応物 4

HCID 795ImidazoleHCID 6344DichloromethaneHCID 24758Sodium hydrideHCID 2759373(3-Iodopropyl)trimethoxysilane

生成物 1

HCID 14419323HCID 14419323、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

5 g (73 mmol) of imidazole were dissolved in 100 ml of tetrahydrofurane and 1.73 g (73 mmol) of sodium hydride were added. The suspension was stirred for 4 hours, after which 10 ml of iodopropyltrimethoxy silane (52 mmol) were added and the reaction mixture was heated under reflux for 18 hours. 15 ml of dichloromethane were then added and the reaction mixture was filtered. The filtrate was concentrated under reduced pressure and the product was distilled off at 150-155° C. at 8 mbar. The yield was 8.2 g (60%).

後処理

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 18 hours
  3. filtrationthe reaction mixture was filtered
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. distillationthe product was distilled off at 150-155° C. at 8 mbar

出典と根拠

ORDレコード
ord-38adc40401b7427a9df5599cad9438fb
出典データセット
uspto-grants-2013_01
特許番号
US08361627B2

反応ノート

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