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Ammonium Chloride → HCID 178420261、化合物

HRID 1415155
ノート
印刷プレビュー

反応式

HRID 1415155 の反応式
[C:1]1([C:7]([C:20]2[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=2)([CH2:10][CH2:11][N:12]2[CH2:17][CH:16]3[CH2:18][CH2:19][CH:13]2[CH2:14][CH2:15]3)[C:8]#[N:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[N-:26]=[N+:27]=[N-:28].[Na+].[Cl-].[NH4+].[Cl-].[Li+]>CN(C)C=O>[C:1]1([C:7]([C:8]2[NH:28][N:27]=[N:26][N:9]=2)([C:20]2[CH:21]=[N:22][CH:23]=[CH:24][CH:25]=2)[CH2:10][CH2:11][N:12]2[CH2:17][CH:16]3[CH2:15][CH2:14][CH:13]2[CH2:19][CH2:18]3)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 433294Lithium ChlorideHCID 203569662-Phenyl-(3-pyridyl)-4-(2-azabicyclo[2.2.2]oct-2-yl)butyronitrile

生成物 1

HCID 178420261HCID 178420261、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
120 °C

実験手順

A mixture of 5.69 parts of 2-phenyl-(3-pyridyl)-4-(2-azabicyclo[2.2.2]oct-2-yl)butyronitrile, 1.67 parts of sodium azide, 1.38 parts of ammonium chloride and 0.025 parts of lithium chloride in 30 parts by volume of dimethylformamide was stirred for 12 hours under nitrogen at 120° C. After the reaction time was completed, the material was cooled and filtered. The collected precipitate was washed with dimethylformamide and water. The precipitate was then dissolved in 100 parts by volume of 0.2N NaOH. The resultant solution was filtered. The filtrates were neutralized with dilute hydrochloric acid. The product which separated was recrystallized from ethanol. The procedure afforded 5-[1-phenyl-1-(3-pyridyl)-3-(2-azabicyclo[2.2.2]oct-2-yl)propyl]-1H-tetrazole.

後処理

  1. temperaturethe material was cooled
  2. filtrationfiltered
  3. washThe collected precipitate was washed with dimethylformamide and water
  4. dissolutionThe precipitate was then dissolved in 100 parts by volume of 0.2N NaOH
  5. filtrationThe resultant solution was filtered
  6. customThe product which separated
  7. customwas recrystallized from ethanol

出典と根拠

ORDレコード
ord-9b8cbecba36f4c6a9d15d7ab3d618bb4
出典データセット
uspto-grants-1977_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04003904

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート