Hydrogen chloride-ethyl acetate → HCID 178485752, compound

HRID 1290075Notes

Reaction equation

HRID 1290075 reaction equation
[CH:1]1([CH2:7][C@H:8]([NH:19][C:20](=[O:49])[C@H:21]([CH2:43][C:44]2[N:48]=[CH:47][NH:46][CH:45]=2)[N:22]([CH3:42])[C:23](=[O:41])[C@H:24]([CH2:34][C:35]2[CH:40]=[CH:39][CH:38]=[CH:37][CH:36]=2)[NH:25][C:26]([N:28]2[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]2)=[O:27])[C@@H:9]([OH:18])[CH2:10][C@H:11]2[C:15]([CH3:17])([CH3:16])[O:14][CH2:13][O:12]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.[ClH:50].C(OCC)(=O)C>C(O)C.C(OCC)(=O)C>[ClH:50].[CH:1]1([CH2:7][C@H:8]([NH:19][C:20](=[O:49])[C@H:21]([CH2:43][C:44]2[N:48]=[CH:47][NH:46][CH:45]=2)[N:22]([CH3:42])[C:23](=[O:41])[C@H:24]([CH2:34][C:35]2[CH:36]=[CH:37][CH:38]=[CH:39][CH:40]=2)[NH:25][C:26]([N:28]2[CH2:33][CH2:32][CH2:31][CH2:30][CH2:29]2)=[O:27])[C@@H:9]([OH:18])[CH2:10][C@H:11]2[C:15]([CH3:17])([CH3:16])[O:14][CH2:13][O:12]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

Participants

5

Reactant 2

HCID 21866389Hydrogen chloride-ethyl acetateHCID 178485751HCID 178485751, compound

Product 1

HCID 178485752HCID 178485752, compound

Reagents, catalysts & solvents 2

HCID 702EthanolSolventHCID 8857Ethyl AcetateSolvent

Procedure

The compound (300 mg) obtained in Example 1 was dissolved in a mixed solution of ethanol (0.27 ml) and ethyl acetate (5.13 ml) and a solution (2.09 ml) of 0.2N HCl-ethyl acetate was dropwise added. After stirring overnight at room temperature, crystals were collected by filtration and dried under reduced pressure to give 160 mg of the title compound as white crystals (see Table 16).

Workup

  1. filtrationcrystals were collected by filtration
  2. customdried under reduced pressure

Sources & evidence

ORD record
ord-be4c5262dd7f4eb88194f8caa7e5fe14
Source dataset
uspto-grants-1998_05
Patent number
US05750696

Reaction notes

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