Hydrochloric Acid → 5-Amino-1-(2-hydroxyethyl)-4-nitrosopyrazole hydrochloride

HRID 1765459

반응식

HRID 1765459 반응식
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]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 80172-HydrazinoethanolHCID 713615623,3-Dimethoxy-2-hydroxyiminopropionitrile

생성물 1

HCID 184268805-Amino-1-(2-hydroxyethyl)-4-nitrosopyrazole hydrochloride수율 94%

시약·촉매·용매 1

HCID 887Methanol용매

반응 조건

온도
67 °C

실험 절차

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.

후처리

  1. customTo a flask having
  2. customan inner volume of 25 ml and equipped with a stirring device
  3. customthe mixture was reacted
  4. customAfter completion of the reaction, when the reaction mixture

출처 및 근거

ORD 기록
ord-5181e8ae4bda4f58be10c7f24ccf6c1a
출처 데이터셋
uspto-grants-2007_06
특허 번호
US07227032B2

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