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Nitric Acid → HCID 178459885, compound

HRID 1953502
Notes
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Reaction equation

HRID 1953502 reaction equation
[CH2:1]([O:4][C:5](=[O:33])[NH:6][C@@H:7]([C:15]([N:17]1[CH2:21][CH2:20][CH2:19][C@H:18]1[C:22](=[O:32])[NH:23][CH2:24][C@H:25]1[CH2:30][CH2:29][C@H:28]([NH2:31])[CH2:27][CH2:26]1)=[O:16])[C:8]([S:11][CH:12]([CH3:14])[CH3:13])([CH3:10])[CH3:9])[CH2:2][CH3:3].[N+:34]([O-:37])([OH:36])=[O:35]>C(O)C>[N+:34]([O-:37])([OH:36])=[O:35].[CH2:1]([O:4][C:5](=[O:33])[NH:6][C@@H:7]([C:15]([N:17]1[CH2:21][CH2:20][CH2:19][C@H:18]1[C:22](=[O:32])[NH:23][CH2:24][C@H:25]1[CH2:26][CH2:27][C@H:28]([NH2:31])[CH2:29][CH2:30]1)=[O:16])[C:8]([S:11][CH:12]([CH3:13])[CH3:14])([CH3:9])[CH3:10])[CH2:2][CH3:3]
ParticipantsProcedureWorkupSources & evidenceReaction notes

Participants

4

Reactant 2

HCID 944Nitric AcidHCID 178459883HCID 178459883, compound

Product 1

HCID 178459885HCID 178459885, compound

Reagents, catalysts & solvents 1

HCID 702EthanolSolvent

Procedure

0.49 g of [(S)-1-[(S)-2-[(trans-4-aminocyclohexylmethyl)carbamoyl]pyrrolidine-1-carbonyl]-2-isopropylthio-2-methylpropyl]carbamic acid propyl ester obtained in Example 1 was dissolved in 5 ml of ethanol, and 1.0 ml of 1N nitric acid was added thereto, followed by stirring at room temperature for 30 minutes. The solvent was distilled off under reduced pressure, and then, 5 ml of toluene was added thereto and then distilled off under reduced pressure. The residue was dried under a reduced pressure of about 10 mmHg at room temperature to obtain 0.56 g of a white amorphous substance.

Workup

  1. distillationThe solvent was distilled off under reduced pressure
  2. addition5 ml of toluene was added
  3. distillationdistilled off under reduced pressure
  4. customThe residue was dried under a reduced pressure of about 10 mmHg at room temperature
  5. customto obtain 0.56 g of a white amorphous substance

Sources & evidence

ORD record
ord-041fa1c4d19a4271aa35e1a3300c8c52
Source dataset
uspto-grants-2000_09
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US06117897

Reaction notes

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On this pageParticipantsProcedureWorkupSources & evidenceReaction notes