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Sodium Azide → 2-Azido-6-(trifluoromethyl)pyridine

HRID 1632120
ノート
印刷プレビュー

反応式

HRID 1632120 の反応式
F[C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([C:8]([F:11])([F:10])[F:9])[N:3]=1.[N-:12]=[N+:13]=[N-:14].[Na+]>CS(C)=O>[N:12]([C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([C:8]([F:11])([F:10])[F:9])[N:3]=1)=[N+:13]=[N-:14]
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

4

反応物 2

HCID 33557Sodium AzideHCID 27365012-Fluoro-6-(trifluoromethyl)pyridine

生成物 1

HCID 133393472-Azido-6-(trifluoromethyl)pyridine収率 71.2%

試薬・触媒・溶媒 1

HCID 679Dimethyl Sulfoxide溶媒

反応条件

温度
80 °C

実験手順

A mixture of 82.5 grams (g) of 2-fluoro-6-(trifluoromethyl)pyridine (0.5 mole), 65 g of sodium azide (1.0 mole) and 400 milliliters (ml) of dimethylsulfoxide (DMSO) was heated to a temperature of 80° C. for 18 hours. The mixture was allowed to cool and then poured into 1500 ml of ice water. This resulting mixture was then extracted 4 times with 300 ml of pentane each time. The pentane extracts were combined, washed with 500 ml of a saturated NaCl solution and dried with MgSO4. The pentane was then carefully evaporated leaving 67 g of the desired 2-azido-6-(trifluoromethyl)pyridine as a light yellow oil having an RI of 1.4771 @25° C.

後処理

  1. temperatureto cool
  2. extractionThis resulting mixture was then extracted 4 times with 300 ml of pentane each time
  3. washwashed with 500 ml of a saturated NaCl solution
  4. dry with materialdried with MgSO4
  5. customThe pentane was then carefully evaporated

出典と根拠

ORDレコード
ord-7c2ea18d086e4449a14490cefb97f66f
出典データセット
uspto-grants-1984_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04474599

反応ノート

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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