Hydrochloric Acid → HCID 73056912, compound

HRID 1055488Notes

Reaction equation

HRID 1055488 reaction equation
[ClH:1].[CH3:2][N:3]([C@@H:11]([CH3:43])[C:12]([NH:14][C@H:15]1[CH2:21][O:20][C:19]2[C:22]([C:26]([F:29])([F:28])[F:27])=[CH:23][CH:24]=[CH:25][C:18]=2[N:17]([CH2:30][C:31]2[C:40]3[C:35](=[CH:36][CH:37]=[CH:38][CH:39]=3)[CH:34]=[CH:33][C:32]=2[CH3:41])[C:16]1=[O:42])=[O:13])C(=O)OC(C)(C)C>CCOCC.CO>[ClH:1].[CH3:2][NH:3][C@@H:11]([CH3:43])[C:12]([NH:14][C@H:15]1[CH2:21][O:20][C:19]2[C:22]([C:26]([F:29])([F:28])[F:27])=[CH:23][CH:24]=[CH:25][C:18]=2[N:17]([CH2:30][C:31]2[C:40]3[C:35](=[CH:36][CH:37]=[CH:38][CH:39]=3)[CH:34]=[CH:33][C:32]=2[CH3:41])[C:16]1=[O:42])=[O:13]

Participants

5

Reactant 2

HCID 313Hydrochloric AcidHCID 90037327HCID 90037327, compound

Product 1

HCID 73056912HCID 73056912, compoundYield 82%

Reagents, catalysts & solvents 2

HCID 887MethanolSolventHCID 3283Diethyl EtherSolvent

Procedure

2 M solution of HCl in Et2O (1.26 mL) was added to a solution of tert-butyl methyl((S)-1-((S)-5-((2-methylnaphthalen-1-yl)methyl)-4-oxo-9-(trifluoromethyl)-2,3,4,5-tetrahydrobenzo[b][1,4]oxazepin-3-ylamino)-1-oxopropan-2-yl)carbamate (66 mg, 113 μmol) in MeOH (400 μL) After 2.5 h the mixture was concentrated, MeCN was added to the residue and the mixture concentrated. The residue was lyophilized from MeCN/H2O to afford the title compound (48 mg, 82%) as a white powder. MS m/z 486 (MH)+

Workup

  1. concentrationwas concentrated
  2. additionMeCN was added to the residue
  3. concentrationthe mixture concentrated

Sources & evidence

ORD record
ord-b8cea70a528348999ea5152c78c9ae62
Source dataset
uspto-grants-2016_07
Patent number
US09394263B2

Reaction notes

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