Hydroxylamine HCl → HCID 86628504、化合物

HRID 546665ノート

反応式

HRID 546665 の反応式
C([O-])(=O)C.[Na+].[Cl-].[OH:7][NH3+:8].[F:9][C:10]1[CH:11]=[C:12]([C:16]2([CH:41]=O)[CH2:21][CH2:20][CH2:19][N:18]3[N:22]=[C:23](/[CH:25]=[CH:26]/[C:27]4[CH:32]=[CH:31][C:30]([N:33]5[CH:37]=[C:36]([CH3:38])[N:35]=[CH:34]5)=[C:29]([O:39][CH3:40])[CH:28]=4)[N:24]=[C:17]23)[CH:13]=[CH:14][CH:15]=1.O.C(=O)(O)[O-].[Na+]>C(O)C.C(OCC)(=O)C>[F:9][C:10]1[CH:11]=[C:12]([C:16]2([CH:41]=[N:8][OH:7])[CH2:21][CH2:20][CH2:19][N:18]3[N:22]=[C:23](/[CH:25]=[CH:26]/[C:27]4[CH:32]=[CH:31][C:30]([N:33]5[CH:37]=[C:36]([CH3:38])[N:35]=[CH:34]5)=[C:29]([O:39][CH3:40])[CH:28]=4)[N:24]=[C:17]23)[CH:13]=[CH:14][CH:15]=1

参加物

7

反応物 4

HCID 21645Hydroxylamine HClHCID 517045Sodium AcetateHCID 86585896Sodium bicarbonate waterHCID 86628503HCID 86628503、化合物

生成物 1

HCID 86628504HCID 86628504、化合物収率 99.8%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Sodium acetate (58.7 mg) and hydroxylammonium chloride (49.8 mg) were added to a solution of 8-(3-fluorophenyl)-2-{(E)-2-[3-methoxy-4-(4-methyl-1H-imidazol-1-yl)phenyl]vinyl}-5,6,7,8-tetrahydro[1,2,4]triazolo[1,5-a]pyridine-8-carbaldehyde (164 mg) in ethanol (10 mL), and the reaction solution was stirred at room temperature for five hours. Ethyl acetate and saturated sodium bicarbonate water were added to the reaction solution and the organic layer was separated. The resulting organic layer was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure to obtain 169 mg of the title compound. The property value of the compound is as follows.

後処理

  1. customthe organic layer was separated
  2. dry with materialThe resulting organic layer was dried over anhydrous magnesium sulfate
  3. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-a5d7231bc73549a08d272da209412952
出典データセット
uspto-grants-2011_05
特許番号
US07935815B2

反応ノート

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