HCID 14003457, compound → HCID 14003467, compound

HRID 569759Notes

Reaction equation

HRID 569759 reaction equation
[ClH:1].O1CCOCC1.[CH2:8]([O:10][C:11]([C@@H:13]([NH:22][C@H:23]1[CH2:29][CH2:28][C@H:27]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH2:26][N:25]([CH2:36][C:37]([O:39]C(C)(C)C)=[O:38])[C:24]1=[O:44])[CH2:14][CH2:15][C:16]1[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=1)=[O:12])[CH3:9]>>[ClH:1].[CH2:8]([O:10][C:11]([C@@H:13]([NH:22][C@H:23]1[CH2:29][CH2:28][C@H:27]([C:30]2[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=2)[CH2:26][N:25]([CH2:36][C:37]([OH:39])=[O:38])[C:24]1=[O:44])[CH2:14][CH2:15][C:16]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=1)=[O:12])[CH3:9]

Participants

3

Reactant 2

HCID 14003457HCID 14003457, compoundHCID 204431481,4-Dioxane hydrochloride

Product 1

HCID 14003467HCID 14003467, compound

Procedure

4 ml of a 4N hydrogen chloride/dioxane solution in which was dissolved 0.95 g of t-butyl α-{3(S)-[1(S)-ethoxycarbonyl-3-phenylpropylamino]-2-oxo-6(R)-phenylperhydroazepin-1-yl}acetate (Isomer A-2) [prepared as described in Example 1(l)] were allowed to stand for 16 hours; at the end of this time, the solvent was distilled off, and the syrupy residue was mixed with a small amount of ethyl acetate and diisopropyl ether and then filtered, to give 0.80 g of the title compound as a crystalline powder, melting at 200°-202° C.

Workup

  1. distillationat the end of this time, the solvent was distilled off
  2. additionthe syrupy residue was mixed with a small amount of ethyl acetate and diisopropyl ether
  3. filtrationfiltered

Sources & evidence

ORD record
ord-a38eec5b21b945e7b29b5a355dbeb157
Source dataset
uspto-grants-1988_03
Patent number
US04734410

Reaction notes

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