Ethyl 3-(hydroxymethyl)-4-(methylamino)pyrrolidine-1-carboxylate → (4-(Methylamino)pyrrolidin-3-yl)methanol
Reaction equation
[OH:1][CH2:2][CH:3]1[CH2:7][N:6](C(OCC)=O)[CH2:5][CH:4]1[NH:13][CH3:14]>O>[OH:1][CH2:2][CH:3]1[CH2:7][NH:6][CH2:5][CH:4]1[NH:13][CH3:14]Participants
3
Reactant 1
Product 1
Reagents, catalysts & solvents 1
Procedure
34 g (0.168 mol) of ethyl 4-hydroxymethyl-3-methylaminopyrrolidine-1-carboxylate are heated under reflux with 100 g of Ba(OH)2.8H2O in 400 ml of water overnight. The BaCO3 is filtered off with suction, the filtrate is concentrated and the residue is boiled up ten times with 100 ml of dioxane each time. The dioxane solutions are filtered, the filtrate is concentrated and the residue is distilled.
Workup
- filtrationThe BaCO3 is filtered off with suction
- concentrationthe filtrate is concentrated
- filtrationThe dioxane solutions are filtered
- concentrationthe filtrate is concentrated
- distillationthe residue is distilled
Sources & evidence
- ORD record
- ord-86770ff2bc704ac38d0ea5db59a975f1
- Source dataset
- uspto-grants-1995_05
- Patent number
- US05416096
Reaction notes
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