HCID 19100973, compound → HCID 19100943, compound

HRID 1975028Notes

Reaction equation

HRID 1975028 reaction equation
[F:1][CH2:2][C:3]12[CH2:10][N:9](C(OCC)=O)[CH2:8][CH:7]1[N:6]([CH3:16])[CH2:5][CH2:4]2>Cl>[F:1][CH2:2][C:3]12[CH2:10][NH:9][CH2:8][CH:7]1[N:6]([CH3:16])[CH2:5][CH2:4]2

Participants

3

Procedure

7.1 g (26 mmol) of ethyl 5-fluoromethyl-2-methyl-2,7-diazabicyclo[3.3.0]octane-7-carboxylate in 100 ml of concentrated hydrochloric acid are refluxed overnight. The mixture is concentrated, the concentrate is taken up in 20 ml of water, this mixture is rendered alkaline using potassium carbonate and extracted ten times using 50 ml portions of chloroform, and the extracts are dried over potassium carbonate, concentrated and distilled.

Workup

  1. concentrationThe mixture is concentrated
  2. extractionextracted ten times
  3. dry with materialthe extracts are dried over potassium carbonate
  4. concentrationconcentrated
  5. distillationdistilled

Sources & evidence

ORD record
ord-15f90691a1d34175a558224d4324b463
Source dataset
uspto-grants-1994_02
Patent number
US05284855

Reaction notes

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