Reaction equation
CCN(C(C)C)C(C)C.[C:10]([Cl:13])(Cl)=[O:11].[CH2:14]([NH:20][CH3:21])[CH2:15][CH2:16][CH2:17][CH2:18][CH3:19]>C(OCC)C>[CH2:14]([N:20]([CH3:21])[C:10]([Cl:13])=[O:11])[CH2:15][CH2:16][CH2:17][CH2:18][CH3:19]Participants
5
Reactant 3
Product 1
Reagents, catalysts & solvents 1
Conditions
- Temperature
- 25 °C
Procedure
To a solution of 0.35 ml of (i-Pr)2NEt in 10 ml of diethyl ether at 0° C. was added phosgene (1.06 ml, 1.93 M solution in toluene) and N-hexylmethylamine (0.31 ml, 2.05 mm). The reaction mixture was allowed to warm up to 25° C., and further stirred at 25° C. for 14 h. The mixture was filtered, and the solvent was removed under vacuum. The product was used for the next step reaction without further purification. 1H NMR (CDCl3): δ 3.42 (m, 2H),.3.07 (s, 3H), 1.59 (m, 2H), 1.31 (m, 6H), 0.90 (m, 3H).
Workup
- filtrationThe mixture was filtered
- customthe solvent was removed under vacuum
- customThe product was used for the next step reaction without further purification
Sources & evidence
- ORD record
- ord-fd0646c8203b474297d9e200d2fd09ee
- Source dataset
- uspto-grants-2007_09
- Patent number
- US07270801B2
Linked notes
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