Sodium Azide → 2,2-Difluoro-2-(2-pyridyl)ethylazide

HRID 398364ノート

反応式

HRID 398364 の反応式
FC(F)(F)S(O[CH2:7][C:8]([F:16])([F:15])[C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=1)(=O)=O.[N-:19]=[N+:20]=[N-:21].[Na+]>CN(C=O)C.O>[F:15][C:8]([F:16])([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][N:10]=1)[CH2:7][N:19]=[N+:20]=[N-:21]

参加物

5

反応物 2

HCID 33557Sodium AzideHCID 110662242,2-Difluoro-2-(2-pyridyl)ethyl trifluoromethanesulfonate

生成物 1

HCID 118054052,2-Difluoro-2-(2-pyridyl)ethylazide

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A solution of 105 mg (0.31 mmol) of 2,2-difluoro-2-(2-pyridyl)ethyl trifluoromethanesulfonate and 43 mg (0.66 mmol) of sodium azide in 1.0 mL of DMF was heated at 60° C. under Ar. After 1.5 h, the mixture was cooled to rt, diluted with water and extracted with two portions of ether. The combined organic layers were washed twice with water, brine and dried over MgSO4. The solvents were removed at reduced pressure and a bath temperature of 20° C. to give the title compound as a brown oil:

後処理

  1. extractionextracted with two portions of ether
  2. washThe combined organic layers were washed twice with water, brine
  3. dry with materialdried over MgSO4
  4. customThe solvents were removed at reduced pressure and a bath temperature of 20° C.

出典と根拠

ORDレコード
ord-28647f88efce40969b6626cf0ac53900
出典データセット
uspto-grants-2003_08
特許番号
US06610692B1

反応ノート

読み込み中…