Methanol → HCID 20230899, compound

HRID 544088Notes

Reaction equation

HRID 544088 reaction equation
[NH2:1][CH2:2][CH2:3][NH:4][CH2:5][CH2:6][NH:7][CH2:8][CH2:9][NH:10][CH2:11][CH2:12][NH2:13].[Si:14]([CH2:21][CH2:22][CH2:23]Cl)([O:19][CH3:20])([O:17][CH3:18])[O:15][CH3:16].[CH3:25][OH:26]>O>[CH3:16][O:15][Si:14]([CH:21]([Si:14]([O:17][CH3:18])([O:15][CH3:16])[O:26][CH3:25])[CH2:22][CH2:23][NH:13][CH2:12][CH2:11][NH:10][CH2:9][CH2:8][NH:7][CH2:6][CH2:5][NH:4][CH2:3][CH2:2][NH2:1])([O:19][CH3:20])[O:17][CH3:18]

Participants

5

Reactant 3

HCID 887MethanolHCID 8197TetraethylenepentamineHCID 624493-(Trimethoxysilyl)propyl chloride

Product 1

HCID 20230899HCID 20230899, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Conditions

Temperature
65 °C

Procedure

In a reaction flask, equipped as in example 1, there was placed 20 gms. (0.1 mole plus 10% mole excess) of tetraethylenepentamine, 40 gms. (0.2 moles) of distilled (CH3O)3Si(CH2)3Cl and 40 gms. of CH3OH. This mixture was refluxed (about 65° C.) for 3 hours where a titration showed 0.07 equiv. of Cl-. The reaction was continued at reflux for an additional 21 hours whereupon the reaction mass titrated at 0.19 equiv. of Cl-. A crude sample of this material (10 weight %) gave an initial hazy solution in acidic water or basic water but the material cleared within about 30 minutes to give stable solutions.

Workup

  1. customIn a reaction flask, equipped as in example 1, there
  2. temperatureat reflux for an additional 21 hours whereupon the reaction mass
  3. customto give stable solutions

Sources & evidence

ORD record
ord-818e965b3677488298f6aef5418e6744
Source dataset
uspto-grants-1984_05
Patent number
US04448694

Reaction notes

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