Hydrochloric Acid → HCID 15018952, compound

HRID 1638927Notes

Reaction equation

HRID 1638927 reaction equation
[Cl:1][C:2]1[C:10]2[O:9][CH:8]([CH3:11])[CH2:7][C:6]=2[C:5]([NH:12][C:13]([N:15]2[CH2:20][CH2:19][CH2:18][CH2:17][CH:16]2[C:21]([O:23]CC)=O)=[O:14])=[CH:4][CH:3]=1.Cl>C(O)C>[Cl:1][C:2]1[C:10]2[O:9][CH:8]([CH3:11])[CH2:7][C:6]=2[C:5]([N:12]2[C:21](=[O:23])[CH:16]3[CH2:17][CH2:18][CH2:19][CH2:20][N:15]3[C:13]2=[O:14])=[CH:4][CH:3]=1

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 54174618HCID 54174618, compound

Product 1

HCID 15018952HCID 15018952, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

A mixture of 2.0 g of 34B, 25 mL of ethanol and 25 mL of 2N hydrochloric acid was stirred and refluxed for 2 hours. Then the solvent was evaporated, the residue was mixed with 50 mL of water, and the resulting mixture was extracted with methylene chloride The extract was dried (MgSO4) and the solvent was evaporated. The residue was purified by filtration through a short pad of silica gel, with a 1:1 v:v mixture ethyl acetate and hexane as eluent, to give the title compound, as a solid, m.p.: 145°-148° C.

Workup

  1. temperaturerefluxed for 2 hours
  2. customThen the solvent was evaporated
  3. additionthe residue was mixed with 50 mL of water
  4. extractionthe resulting mixture was extracted with methylene chloride The extract
  5. dry with materialwas dried (MgSO4)
  6. customthe solvent was evaporated
  7. filtrationThe residue was purified by filtration through a short pad of silica gel, with a 1:1 v

Sources & evidence

ORD record
ord-33d74867c1eb4d73ad3b7be7376e7ca4
Source dataset
uspto-grants-1989_11
Patent number
US04881967

Reaction notes

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