Water → HCID 59398324, compound

HRID 39684Notes

Reaction equation

HRID 39684 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-1a20acba42b44c2fb88c7da546c2a2e8
Source dataset
uspto-grants-2013_09
Patent number
US08524738B2

Reaction notes

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