Hydrochloric Acid → 6-Azidosulfonylhexyltriethoxysilane

HRID 1194067ノート

反応式

HRID 1194067 の反応式
[N-:1]=[N+:2]=[N-:3].[Na+].Cl.[N-]=[N+]=[N-].[CH2:9]([O:11][Si:12]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][S:25](Cl)(=[O:27])=[O:26])([O:16][CH2:17][CH3:18])[O:13][CH2:14][CH3:15])[CH3:10]>P([O-])([O-])(O)=O.[Na+].[Na+].C(Cl)Cl>[CH2:9]([O:11][Si:12]([CH2:19][CH2:20][CH2:21][CH2:22][CH2:23][CH2:24][S:25]([N:1]=[N+:2]=[N-:3])(=[O:27])=[O:26])([O:13][CH2:14][CH3:15])[O:16][CH2:17][CH3:18])[CH3:10]

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 33557Sodium AzideHCID 33558AzideHCID 86742803HCID 86742803、化合物

生成物 1

HCID 220457406-Azidosulfonylhexyltriethoxysilane

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 24203Sodium Phosphate, Dibasic溶媒

実験手順

Sodium azide (1.5 equivalent) in 4 ml of sodium hydrogen phosphate and hydrogen chloride buffer (14.4 g or Na2HPO4 to 4.4 mil conc HCl in 1 liter of distilled water) per gram of azide is added dropwise to a stirred 50 percent solution of triethoxysilylhexane sulfonyl chloride in methylene chloride containing 1 percent Aliquat 336. The mixture is stirred at room temperature for thirty minutes after the addition is complete. The layers are separated. The methylene chloride layer is washed with a saturated salt solution, dried over magnesium sulfate and the methylene chloride is evaporated. Ninety percent solids of a light yellow liquid triethoxysilylhexane sulfonyl azide of about 90 percent purity are obtained.

後処理

  1. additionafter the addition
  2. customThe layers are separated
  3. washThe methylene chloride layer is washed with a saturated salt solution
  4. dry with materialdried over magnesium sulfate
  5. customthe methylene chloride is evaporated

出典と根拠

ORDレコード
ord-9787aeaaecd34093a042e510810e6d2c
出典データセット
uspto-grants-1989_03
特許番号
US04812519

反応ノート

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