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

HRID 990709ノート

反応式

HRID 990709 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. After 1.5 h, the mixture was cooled, 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 to give 1-9 as a brown oil: 1H NMR (CDCl3) δ8.68 (d, 1H, 4.2 Hz), 7.86 (td,1H, 7.8, 1.5 Hz), 7.72 (d, 1H, 7.8 Hz), 7.40-7.45 (m, 1H), 4.03 (t, 2 H, 13.2 Hz).

後処理

  1. temperaturethe mixture was cooled
  2. extractionextracted with two portions of ether
  3. washThe combined organic layers were washed twice with water, brine
  4. dry with materialdried over MgSO4
  5. customThe solvents were removed at reduced pressure

出典と根拠

ORDレコード
ord-decedcd859dc40c395ba0433b53c70d6
出典データセット
uspto-grants-2002_10
特許番号
US06462050B1

反応ノート

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