反应 #3247091
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US04778813
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: A 1000 mL four-neck flask equipped with a reflux condenser, mechanical stirrer, thermometer and a dropping funnel was charged with 149.5 g (1.0 mole) of a 98 percent, N,N,N',N'-tetramethyl-2-hydroxy-1,3-propanediamine. The flask was immersed into an ice-water bath while 197.2 g (2.0 moles) of concentrated hydrochloric acid was introduced at such a rate as to keep the temperature between 35° and 45° C. To the N,N,N',N'-tetramethyl-2-hydroxy-1,3-propanediamine dihydrochloride so obtained, 185.0 g (2.0 moles) of epichlorohydrin was added slowly, taking care that the temperature did not exceed 45° C. After the addition was completed, the temperature was raised to between 60° and 71° C. for 30 minutes. A 77.2 percent solution of the title compound was obtained. A 1000 mL four-neck flask equipped with a reflux condenser, mechanical stirrer was introduced at such a rate as the temperature between 35° and 45° C
来源 ID: ord-415d5e24d68943a5a60d08a22a22ed44