HCID 20660016, compound → HCID 20660014, compound

HRID 1066263Notes

Reaction equation

HRID 1066263 reaction equation
C[O:2][C:3]1[C:4]([CH3:25])=[C:5]([NH:11][C:12](=[O:24])[CH2:13][C:14]23[CH2:23][CH:18]4[CH2:19][CH:20]([CH2:22][CH:16]([CH2:17]4)[CH2:15]2)[CH2:21]3)[CH:6]=[C:7]([O:9]C)[CH:8]=1>C(O)(=O)C>[OH:2][C:3]1[C:4]([CH3:25])=[C:5]([NH:11][C:12](=[O:24])[CH2:13][C:14]23[CH2:23][CH:18]4[CH2:17][CH:16]([CH2:22][CH:20]([CH2:19]4)[CH2:21]2)[CH2:15]3)[CH:6]=[C:7]([OH:9])[CH:8]=1

Participants

3

Reactant 1

HCID 20660016HCID 20660016, compound

Product 1

HCID 20660014HCID 20660014, compound

Reagents, catalysts & solvents 1

HCID 176Acetic AcidSolvent

Procedure

A solution of dimethoxy ether from Example 43 (2.0 g) in 50% hycdrobromic acid in acetic acid was heated at 100 degrees for 12 hours. The solution was concentrated under vacuum, the residue taken in water and extracted with ethyl acetate. The organic layers were dried over magnesium sulfate, filtered, concentrated under vacuum. The crude material was purified over silica eluting with dichloromethane' ethyl acetateto afford the title compound as a white solid.

Workup

  1. concentrationThe solution was concentrated under vacuum
  2. extractionextracted with ethyl acetate
  3. dry with materialThe organic layers were dried over magnesium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under vacuum
  6. customThe crude material was purified over silica eluting with dichloromethane' ethyl

Sources & evidence

ORD record
ord-e894d1d3661743adb4c6d88b97899fb0
Source dataset
uspto-grants-2001_06
Patent number
US06242470B1

Reaction notes

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