Triethanolamine → HCID 58213445, compound
Reaction equation
[N:1]([CH2:8][CH2:9][OH:10])([CH2:5][CH2:6][OH:7])[CH2:2][CH2:3][OH:4].[CH2:11]1[CH2:18][O:17][S:14](=[O:16])(=[O:15])[CH2:13][CH2:12]1>ClCCl>[OH:4][CH2:3][CH2:2][N+:1]([CH2:8][CH2:9][OH:10])([CH2:5][CH2:6][OH:7])[CH2:18][CH2:11][CH2:12][CH2:13][S:14]([O-:17])(=[O:16])=[O:15]Participants
Reactant 2
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 0 °C
Procedure
1.49 grams of triethanolamine was added to a 100 mL round bottom flask equipped with a stir bar. 40 mL of dichloromethane was added to the flask and the mixture stirred thoroughly. The solution was cooled to near 0° C. using an ice water bath. 1.36 grams of 1,4-butanesultone was dissolved in 8 mL of dichloromethane and the butanesultone solution added dropwise to the stirred triethanolamine solution. Following complete addition the ice water bath was removed and the solution allowed to warm to room temperature. The mixture was stirred for 16 hours during which a flocculent precipitate formed. The solid was filtered using a medium porosity glass fritted funnel. The white solid was washed using 30 mL of ethyl ether and the solid dried in a dessicator over Drierite® to give 2.52 grams of a white solid. The structure was confirmed by positive mode electrospray mass spectometry (M+Na)=308.3 m/z and 1H NMR.
Workup
- customequipped with a stir bar
- customwas removed
- temperatureto warm to room temperature
- stirringThe mixture was stirred for 16 hours during which a flocculent precipitate
- customformed
- filtrationThe solid was filtered
- washThe white solid was washed
- dry with materialthe solid dried in a dessicator over Drierite®
Sources & evidence
- ORD record
- ord-38fa14f42e5c4f76874af612e9b02311
- Source dataset
- uspto-grants-2013_08
- Patent number
- US08519125B2
Reaction notes
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