Water → HCID 59398324, compound

HRID 2193057Notes

Reaction equation

HRID 2193057 reaction equation
[O:1]1[C:6]2[CH:7]=[CH:8][C:9]([CH2:11][CH2:12][N:13]3[CH2:18][CH2:17][N:16](C(OC(C)(C)C)=O)[CH2:15][CH:14]3[C:26]([O:28][CH2:29][CH3:30])=[O:27])=[CH:10][C:5]=2[O:4][CH2:3][CH2:2]1.Cl.C(O)C.O>C(OCC)(=O)C>[O:1]1[C:6]2[CH:7]=[CH:8][C:9]([CH2:11][CH2:12][N:13]3[CH2:18][CH2:17][NH:16][CH2:15][CH:14]3[C:26]([O:28][CH2:29][CH3:30])=[O:27])=[CH:10][C:5]=2[O:4][CH2:3][CH2:2]1

Participants

5

Reactant 3

HCID 962WaterHCID 21887872Ethanol hydrochlorideHCID 67538955HCID 67538955, compound

Product 1

HCID 59398324HCID 59398324, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent

Procedure

To 0.60 g of 1-tert-butyl 3-ethyl 4-(2-(2,3-dihydro-1,4-benzodioxin-6-yl)ethyl)piperazine-1,3-dicarboxylate, 12 mL of 10 mol/L hydrogen chloride/ethanol was added, and the mixture was stirred for 2 hours, and then the solvent was removed under reduced pressure. The residue thus obtained was added with water and ethyl acetate. The aqueous layer was separated, ethyl acetate was added thereto, and the resultant solution was adjusted to pH 14 with a 5 mol/L aqueous sodium hydroxide solution. The organic layer was separated and dried over potassium carbonate, and the solvent was removed under reduced pressure to obtain 0.34 g of a brown oily substance, ethyl 1-(2-(2,3-dihydro-1,4-benzodioxin-6-yl)ethyl)piperazine-2-carboxylate.

Workup

  1. customthe solvent was removed under reduced pressure
  2. customThe residue thus obtained
  3. customThe aqueous layer was separated
  4. additionethyl acetate was added
  5. customThe organic layer was separated
  6. dry with materialdried over potassium carbonate
  7. customthe solvent was removed under reduced pressure

Sources & evidence

ORD record
ord-392a42f1636c4745a741d0fe3377579d
Source dataset
uspto-grants-2012_12
Patent number
US08329694B2

Reaction notes

Loading…