Hydroxyammonium hydrochloride → HCID 178513274, 화합물

HRID 708977

반응식

HRID 708977 반응식
Cl[C:2]1[N:7]=[CH:6][C:5]([CH2:8][N+:9]2[C:14]([O-:15])=[C:13]([C:16]3[CH:21]=[CH:20][C:19]([C:22]#[N:23])=[CH:18][CH:17]=3)[C:12](=[O:24])[N:11]3[CH:25]=[CH:26][CH:27]=[CH:28][C:10]=23)=[CH:4][CH:3]=1.[ClH:29].[OH:30][NH3+:31].CC(C)([O-])C.[K+]>CS(C)=O.[Cl-].[Na+].O>[Cl:29][C:2]1[N:7]=[CH:6][C:5]([CH2:8][N+:9]2[C:14]([O-:15])=[C:13]([C:16]3[CH:21]=[CH:20][C:19]([C:22](=[NH:23])[NH:31][OH:30])=[CH:18][CH:17]=3)[C:12](=[O:24])[N:11]3[CH:25]=[CH:26][CH:27]=[CH:28][C:10]=23)=[CH:4][CH:3]=1

참가 물질

6

반응물 3

HCID 22029257Hydroxyammonium hydrochlorideHCID 23665647Potassium tert-butoxideHCID 867092651-[(6-Chloro-3-pyridyl)methyl]-3-(4-cyanophenyl)-4-oxo-pyrido[1,2-a]pyrimidin-1-ium-2-olate2회

생성물 1

HCID 178513274HCID 178513274, 화합물

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 57417360Sodium chloride; water용매

실험 절차

30 mg (0.08 mmol) of 1-[(6-chloro-3-pyridyl)methyl]-3-(4-cyanophenyl)-4-oxo-pyrido[1,2-a]pyrimidin-1-ium-2-olate (product of step 1) were dissolved in 2 ml DMSO. 13 mg (0.2 mmol) hydroxylammonium hydrochloride and 22 mg (0.2 mmol) potassium t-butoxide were added and the mixture was stirred at room temperature for 18 hours. The mixture was taken up with 10 ml of brine and extracted with ethyl acetate. The organic phases were dried with magnesium chloride and the solvent was removed under reduced pressure. The desired product was sufficiently pure without further purification (10 mg).

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic phases were dried with magnesium chloride
  3. customthe solvent was removed under reduced pressure
  4. customThe desired product was sufficiently pure without further purification (10 mg)

출처 및 근거

ORD 기록
ord-19999677997c4cac96f8ae74ea9116a4
출처 데이터셋
uspto-grants-2015_11
특허 번호
US09179680B2

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