Water → HCID 19836661, compound

HRID 476887Notes

Reaction equation

HRID 476887 reaction equation
Cl[C:2]([O:4][CH2:5][CH:6]=[CH2:7])=[O:3].[CH3:8][N:9]1[CH2:14][CH2:13][NH:12][CH2:11][CH2:10]1.O.[OH-].[Na+]>ClCCl>[CH2:5]([O:4][C:2]([N:12]1[CH2:13][CH2:14][N:9]([CH3:8])[CH2:10][CH2:11]1)=[O:3])[CH:6]=[CH2:7]

Participants

6

Reactant 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 18052Allyl chloroformateHCID 531671-Methylpiperazine

Product 1

HCID 19836661HCID 19836661, compound

Reagents, catalysts & solvents 1

HCID 6344DichloromethaneSolvent

Procedure

A solution of allyl chloroformate (15 ml) in dry dichloromethane was added at -20° C. under stirring to a solution of N-methylpiperazine (10 g) in the same solvent. After 30 minutes the temperature was let rise to +15° C. and the reaction mixture was poured into water. The organic layer was discarded, 1N NaOH was added to a pH≥7, and the mixture was extracted with dichloromethane. The CH2Cl2 extracts were dried (MgSO4), evaporated, and the resulting oil distilled 118° C. (at 18 mmHg) to yield 4-allyloxycarbonyl-1-methylpiperazine (15.3 g).

Workup

  1. extractionthe mixture was extracted with dichloromethane
  2. dry with materialThe CH2Cl2 extracts were dried (MgSO4)
  3. customevaporated
  4. distillationthe resulting oil distilled 118° C. (at 18 mmHg)

Sources & evidence

ORD record
ord-15f186a74fdf4ace8e50dab36c20cdbb
Source dataset
uspto-grants-1989_12
Patent number
US04886793

Reaction notes

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