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Trityl chloride → HCID 22915640、化合物

HRID 1377968
ノート
印刷プレビュー

反応式

HRID 1377968 の反応式
[CH3:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([C:12]1[CH:19]=[CH:18][CH:17]=[CH:16][C:13]=1[C:14]#[N:15])[CH:6]=[CH:5]2.[N-:20]=[N+:21]=[N-:22].[Na+].C([Sn](Cl)(CCCC)CCCC)CCC.[OH-].[Na+].[C:40](Cl)([C:53]1[CH:58]=[CH:57][CH:56]=[CH:55][CH:54]=1)([C:47]1[CH:52]=[CH:51][CH:50]=[CH:49][CH:48]=1)[C:41]1[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=1>C1(C)C=CC=CC=1.CCCCCC>[CH3:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([C:12]1[CH:19]=[CH:18][CH:17]=[CH:16][C:13]=1[C:14]1[N:20]=[N:21][N:22]([C:40]([C:41]3[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=3)([C:53]3[CH:54]=[CH:55][CH:56]=[CH:57][CH:58]=3)[C:47]3[CH:48]=[CH:49][CH:50]=[CH:51][CH:52]=3)[N:15]=1)[CH:6]=[CH:5]2
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 5

HCID 6456Trityl chlorideHCID 14798Sodium HydroxideHCID 15096Tributyltin ChlorideHCID 33557Sodium AzideHCID 218042392-(6-Methylquinolin-2-yl)benzonitrile

生成物 1

HCID 22915640HCID 22915640、化合物収率 377.6%

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒2 回HCID 8058Hexane溶媒

実験手順

3.5 ml of toluene were added to 855 mg (3.5 mmol) of 2-(6-methyl-quinolin-2-yl)benzonitrile obtained in Reference Example 8. To the mixture were further added 0.24 g (0.68 mmol) of sodium azide and 1 ml (3.83 mmol) of tributyltin chloride. After heating under reflux for 45 hours, the mixture was allowed to cool and diluted with 7 ml of toluene. To the mixture were added 0.4 ml (4 mmol) of a 10 N sodium hydroxide aqueous solution and 1.01 g (3.61 mmol) of tritylchloride with stirring. After stirring at room temperature for 1.5 hours, 15 ml of hexane were added to the mixture and the solid material was collected by filtration. The thus obtained solid material was washed with 10 ml of water twice and then 5 mls of methanol three times. The filter cake was dried under vacuum to obtain 1.36 g of 5-[2-(6-methylquinolin-2-yl)phenyl]-2-triphenylmethyl-2H-tetrazole.

後処理

  1. customobtained in Reference Example 8
  2. temperatureAfter heating
  3. temperatureunder reflux for 45 hours
  4. temperatureto cool
  5. stirringAfter stirring at room temperature for 1.5 hours
  6. filtrationthe solid material was collected by filtration
  7. washThe thus obtained solid material was washed with 10 ml of water twice
  8. customThe filter cake was dried under vacuum

出典と根拠

ORDレコード
ord-e204673f90424b41a049e40eaead717b
出典データセット
uspto-grants-1997_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05665881

反応ノート

読み込み中…

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