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24th June 2013 @ 07:53

2-bromo-2-methylpropionamide (97% yield) was synthesised from 2-bromoisobutyryl bromide.

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Synthesis of 2-bromo-2-methylpropionamide from 2-bromoisobutyryl bromide. To be used in investigating silver oxide coupling of tertiary alkylbromides with alcohols.

 

 

Reaction start time: 5:00 PM EST 24/6/13

2-bromoisobutyryl bromide (0.42 mL, 0.78 g, 0.39 mmol, 1 equiv.) was stirred in hexane (5 mL) at 0°C, to the mixture was added ammonium hydroxide (0.8 mL, 0.39 mmol, 1 equiv.) as 6 portions divided over 30 minutes. The reaction was stirred for another 30 minutes. A white percipitate formed, which was filtered and washed with cold water. A powdery white solid (0.34 g, 0.36 mmol, 97% yield).

 

Characterisation: 1H-NMR(300MHz, CDCl3): δ 1.97(s, 6H), 5.71(brs, 1H), 6.61(brs, 1H). M.P. of 150°C - 153°C, matched literature values.

 

NMR:

HNMR MD 33-1.pdf

MD_33-1.rar


See also:

1. 2-bromo-2-methylpropionamide HNMR


Risk and Hazard Assessment:

MD 33-1.pdf

Attached Files
24th June 2013 @ 07:45

Formation of methyl ester sulfonamide as a step towards forming 2-(1-(4-fluorophenyl)-2,5-dimethyl-1H-pyrrole-3-sulfonamido)acetate, a possible antimalarial.

Reaction start time: 2:00 PM EST 18/6/13


Risk and Hazard Assessment:

Same as second half of Synthesis of 2-(1-(4-fluorophenyl)-2,5-dimethyl-1H-pyrrole-3-sulfonamido)acetamide (MD 26-2)

24th June 2013 @ 07:27
Formation of sulfonyl chloride intermediate to be used to form a sulfonamide

 

Reaction start time: 11:00 AM EST, 17/6/13



Risk and Hazard Assessment:


Same as Chlorination of sodium 1-(4-fluorophenyl)-2,5-dimethyl-1H-pyrrole-3-sulfonate using oxalyl chloride (MD 27-1)

9th May 2013 @ 08:35

Formation of a sulfonate as an alternative to the sulfonamides (MD 29-1)

Reaction start time: 7:30 PM EST, 9/5/13

MD 27-5 (65 mg, 0.23 mmol, 1 equiv.) was dissolved in pyridine (5 mL). Methyl glycolate (102 mg, 1.1 mmol, 4.9 equiv.) was added and the reaction stirred overnight.

 

 NMR: 

MD 32-1.pdf
MD_32-1.rar


Risk and Hazard assessment:

Attached Files
8th May 2013 @ 04:22
Formation of sulfonyl chloride intermediate to be used to form a sulfonamide
 

Reaction start time: 1:30 PM EST, 8/5/13

MD 6-7 (0.11 g, 0.18 mmol, 1 equiv.) was stirred in dry DCM (3 mL) followed by addition of dry DMF (14 uL, 0.18 mmol, 1 equiv.). Dropwise oxalyl chloride (0.14 mL, 1.6 mmol, 8 equiv.). The reaction mixture was stirred at room temperature for 3 hours.

 

Risk and Hazard assessment:
Chlorination of sodium 1-(4-fluorophenyl)-2,5-dimethyl-1H-pyrrole-3-sulfonate using oxalyl chloride (MD 27-1)