Hydrochloric Acid → HCID 13588532, compound

HRID 1031068Notes

Reaction equation

HRID 1031068 reaction equation
Cl.C([O:6][C:7]([NH:9][CH:10]([C:24]([O:26][CH2:27][CH3:28])=[O:25])[CH2:11][C:12](=[CH2:23])[CH2:13][CH:14]([NH:20]C=O)[C:15]([O:17][CH2:18][CH3:19])=[O:16])=O)(C)(C)C>CCOCC.C(Cl)Cl>[NH2:20][CH:14]([CH2:13][C:12](=[CH2:23])[CH2:11][CH:10]([NH:9][CH:7]=[O:6])[C:24]([O:26][CH2:27][CH3:28])=[O:25])[C:15]([O:17][CH2:18][CH3:19])=[O:16]

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 13588531HCID 13588531, compound

Product 1

HCID 13588532HCID 13588532, compound

Reagents, catalysts & solvents 2

HCID 3283Diethyl EtherSolventHCID 6344DichloromethaneSolvent

Procedure

100 ml of a solution of 2.6N hydrochloric acid in anhydrous ether were added to a solution of 6.4 g of the product of Step F in 200 ml of methylene chloride and after stirring at room temperature for one hour, nitrogen was bubbled therethrough The mixture was evaporated to dryness under reduced pressure at 30° C. and the residue was taken up in methylene chloride. The mixture was neutralized and evaporated to dryness to obtain 4.6 g of raw product. The latter was chromatographed over silica and eluted with a 9-1 ethyl acetate-ethanol mixture to obtain the desired product with an Rf=0.06.

Workup

  1. customnitrogen was bubbled
  2. customThe mixture was evaporated to dryness under reduced pressure at 30° C.
  3. customevaporated to dryness
  4. customto obtain 4.6 g of raw product
  5. customThe latter was chromatographed over silica
  6. washeluted with a 9-1 ethyl acetate-ethanol mixture

Sources & evidence

ORD record
ord-b50594c4e01f40b0bc839485cfc844cc
Source dataset
uspto-grants-1992_04
Patent number
US05108990

Reaction notes

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