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

HRID 398364노트

반응식

HRID 398364 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. 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:

후처리

  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.

출처 및 근거

ORD 기록
ord-28647f88efce40969b6626cf0ac53900
출처 데이터셋
uspto-grants-2003_08
특허 번호
US06610692B1

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