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

HRID 990709노트

반응식

HRID 990709 반응식
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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-decedcd859dc40c395ba0433b53c70d6
출처 데이터셋
uspto-grants-2002_10
특허 번호
US06462050B1

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