Hydrochloric Acid → HCID 70430209, compound

HRID 979834Notes

Reaction equation

HRID 979834 reaction equation
[CH2:1]([O:3][C:4](=[O:23])[CH2:5][C@@H:6]1[CH2:10][CH2:9][CH2:8][N:7]1[C:11](=[O:22])[C@H:12]([CH3:21])[NH:13]C(OC(C)(C)C)=O)[CH3:2].[ClH:24]>C(OCC)(=O)C>[ClH:24].[CH2:1]([O:3][C:4](=[O:23])[CH2:5][C@@H:6]1[CH2:10][CH2:9][CH2:8][N:7]1[C:11](=[O:22])[C@H:12]([CH3:21])[NH2:13])[CH3:2]

Participants

4

Reactant 2

HCID 313Hydrochloric AcidHCID 54243617HCID 54243617, compound

Product 1

HCID 70430209HCID 70430209, compound

Reagents, catalysts & solvents 1

HCID 8857Ethyl AcetateSolvent2×

Procedure

To the product of Step C above (1.125 g) in 3 ml of ethyl acetate at 0° C. was added 6 ml of 5.8M hydrogenchloride in ethyl acetate, an the mixture was kept at 0° C. for 45 minutes. It was then concentrated to dryness; ether (20 ml) was added, and the crystalline hydrochloride salt was collected by filtration and washed with ether: 715 mg (80%) m.p. 175°-8° C.; TLC Rf =0.47 silica gel 4:1:1-n-butanol:water:acetic acid.

Workup

  1. concentrationIt was then concentrated to dryness
  2. additionether (20 ml) was added
  3. filtrationthe crystalline hydrochloride salt was collected by filtration
  4. washwashed with ether

Sources & evidence

ORD record
ord-05d71fc81fb14354898cd3355e03a1d5
Source dataset
uspto-grants-1987_01
Patent number
US04634716

Reaction notes

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