Water → 77278-41-2

HRID 1389994Notes

Reaction equation

HRID 1389994 reaction equation
C([O:9][N:10]1[CH2:15][CH2:14][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:12][CH2:11]1)(=O)C1C=CC=CC=1.C[O-].[Na+].O>CO>[OH:9][N:10]1[CH2:11][CH2:12][N:13]([C:16]([O:18][C:19]([CH3:22])([CH3:21])[CH3:20])=[O:17])[CH2:14][CH2:15]1

Participants

5

Procedure

A solution of 3.8 g (0.012 mole) 1-benzoyloxy-4-[1,1-dimethylethoxycarbonyl]piperazine in 25 ml methanol-ether (1:1) was added dropwise to a stirred suspension of 0.95 g (0.017 mole) sodium methoxide in 25 ml methanol at room temperature. The mixture was stirred for 2 hours, treated with 50 ml H2O, and evaporated in vacuo. The residue was thoroughly extracted with ether and the extracts were dried (MgSO4), filtered, diluted with hexane, and evaporated to a lower volume to yield 1.9 white, crystalline solid, m.p. 95°-97° C. Calc. for C9H18N2O3 (202.25): C, 53.45; H, 8.97; N, 13.85; O, 23.73. Found: C, 53.26; H, 8.74; N, 13.98; O, 23.96.

Workup

  1. customevaporated in vacuo
  2. extractionThe residue was thoroughly extracted with ether
  3. dry with materialthe extracts were dried (MgSO4)
  4. filtrationfiltered
  5. additiondiluted with hexane
  6. customevaporated to a lower volume
  7. customto yield 1.9 white

Sources & evidence

ORD record
ord-94bf5719681a4e8e8a7be5e850929b3b
Source dataset
uspto-grants-1981_01
Patent number
US04247549

Reaction notes

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