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HCID 178466979、化合物 → HCID 178433885、化合物

HRID 555620
ノート
印刷プレビュー

反応式

HRID 555620 の反応式
[C:1]([C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C:15]([OH:16])=[C:14]([C:17](=O)[CH3:18])[C:13]([CH3:20])=[N:12]2)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2].[NH:21]1[C:25]([C:26]2[CH:35]=[CH:34][C:29]([C:30]([NH:32][NH2:33])=[O:31])=[CH:28][CH:27]=2)=[N:24][N:23]=[N:22]1>Cl.CN(C=O)C>[C:1]([C:5]1[CH:10]=[CH:9][C:8]([N:11]2[C:15](=[O:16])[C:14](=[C:17]([NH:33][NH:32][C:30](=[O:31])[C:29]3[CH:34]=[CH:35][C:26]([C:25]4[NH:24][N:23]=[N:22][N:21]=4)=[CH:27][CH:28]=3)[CH3:18])[C:13]([CH3:20])=[N:12]2)=[CH:7][CH:6]=1)([CH3:4])([CH3:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 178466979HCID 178466979、化合物HCID 178514418HCID 178514418、化合物

生成物 1

HCID 178433885HCID 178433885、化合物収率 12.9%

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid触媒HCID 6228Dimethylformamide溶媒

実験手順

A DMF solution (1 ml) of 27.2 mg (0.10 mmol) of 1-(1-(4-tert-butylphenyl)-5-hydroxy-3-methyl-1H-pyrazol-4-yl)-ethanone and 20.4 mg (0.10 mmol) of 4-(1H-tetrazol-5-yl)-benzoic hydrazide synthesized by the method disclosed in WO03/037328 was heated at 60° C. for 6 hours with one drop of concentrated hydrochloric acid, and the precipitated solid was washed with water and collected by filtration. The solid was mixed with 1M aqueous sodium hydroxide and filtered. 1M Hydrochloric acid was added to the filtrate, and the precipitated solid was collected by filtration to obtain 5.9 mg of the desired product as a brown solid (yield 12%).

後処理

  1. washthe precipitated solid was washed with water
  2. filtrationcollected by filtration
  3. additionThe solid was mixed with 1M aqueous sodium hydroxide
  4. filtrationfiltered
  5. addition1M Hydrochloric acid was added to the filtrate
  6. filtrationthe precipitated solid was collected by filtration

出典と根拠

ORDレコード
ord-d0a6d0a2256f437bb85a3aa71904c89e
出典データセット
uspto-grants-2011_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08053453B2

反応ノート

読み込み中…

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