Triethylamine → HCID 21701670, compound

HRID 1596225Notes

Reaction equation

HRID 1596225 reaction equation
Cl.Cl.[C:3]([N:6]1[CH2:11][CH2:10][N:9]([NH2:12])[CH2:8][CH2:7]1)(=[O:5])[CH3:4].C(N(CC)CC)C.Cl[C:21]([O:23][C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)=[O:22]>ClCCl>[C:3]([N:6]1[CH2:11][CH2:10][N:9]([NH:12][C:21](=[O:22])[O:23][C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH2:8][CH2:7]1)(=[O:5])[CH3:4]

Participants

5

Reactant 3

HCID 8471TriethylamineHCID 15891Phenyl chloroformateHCID 21701657HCID 21701657, compound

Product 1

HCID 21701670HCID 21701670, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

To a solution of 1-acetyl-4-aminopiperazine dihydrochloride (300 mg) in dichloromethane (9 ml) was added triethylamine (0.77 ml) and phenyl chloroformate (0.261 ml) at ambient temperature. The mixture was stirred at the same temperature for 1 hour, and washed with water (×2). The organic layer was separated, dried over magnesium sulfate, and concentrated. The residue was crystallized from ethyl acetate and diethyl ether to give phenyl N-(4-acetyl-1-piperazinyl)carbamate (0.29 g).

Workup

  1. washwashed with water (×2)
  2. customThe organic layer was separated
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated
  5. customThe residue was crystallized from ethyl acetate and diethyl ether

Sources & evidence

ORD record
ord-4ca3773b70cf42968dfe4220ad17cd9a
Source dataset
uspto-grants-2001_09
Patent number
US06291464B1

Reaction notes

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