HCID 19100973, compound → HCID 19100943, compound

HRID 1590153Notes

Reaction equation

HRID 1590153 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-41c40c9d8d41407098c78aa1908f7c6b
Source dataset
uspto-grants-1993_04
Patent number
US05202337

Reaction notes

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