Hydroxyammonium hydrochloride → HCID 178513274、化合物

HRID 708977

反応式

HRID 708977 の反応式
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

参加物

6

反応物 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-olate2 回

生成物 1

HCID 178513274HCID 178513274、化合物

試薬・触媒・溶媒 2

HCID 679Dimethyl Sulfoxide溶媒HCID 57417360Sodium chloride; water溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-19999677997c4cac96f8ae74ea9116a4
出典データセット
uspto-grants-2015_11
特許番号
US09179680B2

関連ノート

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