Hydrochloric Acid → 5-Amino-1-(2-hydroxyethyl)-4-nitrosopyrazole hydrochloride
Reaction equation
CO[CH:3](OC)[C:4](=[N:7][OH:8])[C:5]#[N:6].[OH:11][CH2:12][CH2:13][NH:14][NH2:15].[ClH:16]>CO>[ClH:16].[NH2:6][C:5]1[N:14]([CH2:13][CH2:12][OH:11])[N:15]=[CH:3][C:4]=1[N:7]=[O:8]Participants
Conditions
- Temperature
- 67 °C
Procedure
To a flask having an inner volume of 25 ml and equipped with a stirring device, a thermometer and a reflux condenser were charged 1.47 g (10.0 mmol) of 3,3-dimethoxy-2-hydroxyiminopropionitrile with a purity of 98.1% by weight synthesized in the same manner as in Example 1, 0.84 g (10.5 mmol) of 2-hydroxyethylhydrazine with a purity of 95% by weight, 10 ml of methanol and 1.5 ml (18.0 mmol) of conc. hydrochloric acid, and the mixture was reacted under reflux (67° C.) for 1.5 hours. After completion of the reaction, when the reaction mixture was analyzed by high performance liquid chromatography (absolute calibration curve method), it was found that 1.81 g of 5-amino-1-(2-hydroxyethyl)-4-nitrosopyrazole hydrochloride (Reaction yield: 93.8%) had been formed.
Workup
- customTo a flask having
- customan inner volume of 25 ml and equipped with a stirring device
- customthe mixture was reacted
- customAfter completion of the reaction, when the reaction mixture
Sources & evidence
- ORD record
- ord-5181e8ae4bda4f58be10c7f24ccf6c1a
- Source dataset
- uspto-grants-2007_06
- Patent number
- US07227032B2
Reaction notes
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