Potassium Carbonate → 2,2-Dimethyl-3-(Pyrrolidin-1-Yl)Propan-1-Ol

HRID 272850Notes

Reaction equation

HRID 272850 reaction equation
[NH:1]1[CH2:5][CH2:4][CH2:3][CH2:2]1.C([O-])([O-])=O.[K+].[K+].Br[CH2:13][C:14]([CH3:18])([CH3:17])[CH2:15][OH:16]>>[CH3:13][C:14]([CH3:18])([CH2:17][N:1]1[CH2:5][CH2:4][CH2:3][CH2:2]1)[CH2:15][OH:16]

Participants

4

Procedure

Pyrrolidine (1.82 g, 25 mmol), K2CO3 (3.0 g, 1.04 eq.), 3-bromo-2,2-dimethyl-propan-1-ol (8.45 g, 50 mmol, 2 eq.) were heated together at 90° C. overnight. The reaction was allowed to cool to room temperature and quenched with 2M HCl solution (50 ml) and extracted with TBME (3×50 ml). The aqueous phase was basified to pH 14 with 2M NaOH solution and extracted with DCM (3×50 ml). The combined organic extracts were dried over MgSO4, filtered, washed with DCM and concentrated in vacuo to give the title compound (1.03 g, 26%) as a pale yellow oil.

Workup

  1. customquenched with 2M HCl solution (50 ml)
  2. extractionextracted with TBME (3×50 ml)
  3. extractionextracted with DCM (3×50 ml)
  4. dry with materialThe combined organic extracts were dried over MgSO4
  5. filtrationfiltered
  6. washwashed with DCM
  7. concentrationconcentrated in vacuo

Sources & evidence

ORD record
ord-ee5650e5395444e383efec72dc87b728
Source dataset
uspto-grants-2008_11
Patent number
US07456164B2

Reaction notes

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