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Formaldehyde → (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]pyridin-8-yl)methanol

HRID 546663
ノート
印刷プレビュー

反応式

HRID 546663 の反応式
C=O.[H-].[Na+].[F:5][C:6]1[CH:7]=[C:8]([CH:12]2[CH2:17][CH2:16][CH2:15][N:14]3[N:18]=[C:19](/[CH:21]=[CH:22]/[C:23]4[CH:28]=[CH:27][C:26]([N:29]5[CH:33]=[C:32]([CH3:34])[N:31]=[CH:30]5)=[C:25]([O:35][CH3:36])[CH:24]=4)[N:20]=[C:13]23)[CH:9]=[CH:10][CH:11]=1.O.[C:38](=O)(O)[O-:39].[Na+]>CN(C=O)C.C(OCC)(=O)C>[F:5][C:6]1[CH:7]=[C:8]([C:12]2([CH2:38][OH:39])[CH2:17][CH2:16][CH2:15][N:14]3[N:18]=[C:19](/[CH:21]=[CH:22]/[C:23]4[CH:28]=[CH:27][C:26]([N:29]5[CH:33]=[C:32]([CH3:34])[N:31]=[CH:30]5)=[C:25]([O:35][CH3:36])[CH:24]=4)[N:20]=[C:13]23)[CH:9]=[CH:10][CH:11]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 712FormaldehydeHCID 24758Sodium hydrideHCID 25212802HCID 25212802、化合物HCID 86585896Sodium bicarbonate water

生成物 1

HCID 66839396(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]pyridin-8-yl)methanol

試薬・触媒・溶媒 2

HCID 6228
Dimethylformamide
溶媒
HCID 8857Ethyl Acetate溶媒

実験手順

Paraformaldehyde (186 mg) and sodium hydride (containing 40% of mineral oil, 28.7 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 synthesized by the method in Examples 1 and 2 (154 mg) in DMF (3 mL), and the reaction solution was stirred at room temperature for 30 minutes. Thereafter, 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 concentrated under reduced pressure to obtain 204 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-3e354777320b4186bb0a274837d7adda
出典データセット
uspto-grants-2011_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07935815B2

反応ノート

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