Dichloromethane → HCID 178503002、化合物

HRID 1808671ノート

反応式

HRID 1808671 の反応式
[NH:1]1[CH:5]=[N:4][CH:3]=[N: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:5]1[N:4]=[CH:3][NH:2][N:1]=1)([O:17][CH3:18])[O:15][CH3:16]

参加物

6

反応物 4

HCID 6344DichloromethaneHCID 92571H-1,2,4-TriazoleHCID 24758Sodium hydrideHCID 2759373(3-Iodopropyl)trimethoxysilane

生成物 1

HCID 178503002HCID 178503002、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

5 g (72 mmol) of 1,2,4-triazole were dissolved in 100 ml of absolute tetrahydrofurane and 1.73 g (72 mmol) of sodium hydride were added. The reaction mixture 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. 20 ml of dichloromethane were then added and the reaction mixture was filtered. The solvent was removed at 150-155° C. under reduced pressure (8 mbar) and then filtered. The yield was 6.4 g (50%).

後処理

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 18 hours
  3. filtrationthe reaction mixture was filtered
  4. customThe solvent was removed at 150-155° C. under reduced pressure (8 mbar)
  5. filtrationfiltered

出典と根拠

ORDレコード
ord-b9122c1815fe44b389e2c94b1dfb185b
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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