Author Topic: Some questions about synth of DPT  (Read 1724 times)

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hihiyaya

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Some questions about synth of DPT
« on: November 02, 2004, 03:54:00 AM »
Sorry my poor English and I am a new bee
Reading TiHKAL synth of DPT from indole,

http://www.erowid.org/library/books_online/tihkal/tihkal09.shtml


I have some question:
(Q1) There was then added an excess of 2N HCl, the mixture cooled, and the resulting solids removed by filtration.

Which we want to recrystallize ,precipitate or filtrate?

(Q2)Can I exchange dioxane with anhydrous THF?

(Q3) 19 g LAH in 350 mL dioxane which was well stirred and held at reflux temperature under an inert atmosphere

What degree is reflux temperature? And what is inert atmosphere?

(Q4) the excess hydride destroyed by the cautious addition of wet dioxane.

Can I exchange wet dioxane with chips of ice?

(Q5) The brownish residue was dissolved in anhydrous Et2O and saturated with anhydrous hydrogen chloride.

HCL gas is trouble for me.Can I use HCL solution,and then water is distilled away?
:)  :)  :)

Lilienthal

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(Q1) There was then added an excess of 2N HCl,
« Reply #1 on: November 02, 2004, 09:20:00 AM »
(Q1) There was then added an excess of 2N HCl, the mixture cooled, and the resulting solids removed by filtration.
Which we want to recrystallize ,precipitate or filtrate?
(A1) The solid

(Q2)Can I exchange dioxane with anhydrous THF?
(A2) Only if you increase reaction time, the higher the temperature the faster the reaction

(Q3) 19 g LAH in 350 mL dioxane which was well stirred and held at reflux temperature under an inert atmosphere
What degree is reflux temperature? And what is inert atmosphere?
(A3) Reflux temperature = boiling point of the solvent = 101 °C

(Q4) the excess hydride destroyed by the cautious addition of wet dioxane.
Can I exchange wet dioxane with chips of ice?
(A4) That's dangerous, add dioxane-diluted water or small drops of water or conc. MgSO4 solution

(Q5) The brownish residue was dissolved in anhydrous Et2O and saturated with anhydrous hydrogen chloride.
HCL gas is trouble for me.Can I use HCL solution,and then water is distilled away?
(A5) No, your product dissolves in the water phase. Make your HCl in a small generator.