Triethylamine → HCID 21701702, compound

HRID 1596207Notes

Reaction equation

HRID 1596207 reaction equation
[N:1]([N:3]1[CH2:9][CH2:8][CH2:7][NH:6][CH2:5][CH2:4]1)=[O:2].C(N(CC)CC)C.[CH2:17]([O:24][C:25](Cl)=[O:26])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1>ClCCl.O>[CH2:17]([O:24][C:25]([N:6]1[CH2:7][CH2:8][CH2:9][N:3]([N:1]=[O:2])[CH2:4][CH2:5]1)=[O:26])[C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1

Participants

6

Reactant 3

HCID 8471TriethylamineHCID 10387Benzyl chloroformateHCID 427992HCID 427992, compound

Product 1

HCID 21701702HCID 21701702, compound

Reagents, catalysts & solvents 2

HCID 962WaterSolventHCID 6344DichloromethaneSolvent

Procedure

To a stirred solution of 1-nitrosohomopiperazine (4.174 g) and triethylamine (9 ml) in dichloromethane (25 ml) was added dropwise benzyloxycarbonyl chloride (5 ml) at 0° C. The reaction mixture was stirred at ambient temperature for 1 hour. The reaction mixture was diluted with water and separated. The organic layer was washed with water (×2), brine, dried over magnesium sulfate and concentrated to give 1-benzyloxycarbonyl-4-nitrosohomopiperazine (6.0 g). This product was used for the next step without purification.

Workup

  1. customseparated
  2. washThe organic layer was washed with water (×2), brine
  3. dry with materialdried over magnesium sulfate
  4. concentrationconcentrated

Sources & evidence

ORD record
ord-3d560b645bc842d0822520a2c90a71d2
Source dataset
uspto-grants-2001_09
Patent number
US06291464B1

Reaction notes

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