Triethylamine → HCID 67258204, 화합물

HRID 2371042노트

반응식

HRID 2371042 반응식
[Br:1][C:2]1[S:3][CH:4]=[CH:5][C:6]=1[CH:7](O)[CH2:8][N+:9]([O-:11])=[O:10].CCN(CC)CC.CS(Cl)(=O)=O>CN(C1C=CN=CC=1)C.C(Cl)Cl.O>[Br:1][C:2]1[S:3][CH:4]=[CH:5][C:6]=1/[CH:7]=[CH:8]/[N+:9]([O-:11])=[O:10]

참가 물질

7

반응물 3

HCID 8471TriethylamineHCID 31297Methanesulfonyl chlorideHCID 67256195HCID 67256195, 화합물

생성물 1

HCID 67258204HCID 67258204, 화합물수율 89%

시약·촉매·용매 3

HCID 142844-(Dimethylamino)pyridine촉매HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

To a solution of 1-(2-bromothiophen-3-yl)-2-nitroethanol (3 g, 12.0 mmol), DMAP (146 mg, 1.2 mmol) and Et3N (2.4 g, 24.0 mmol) in DCM (30 mL) was added MsCl (2.4 g, 24.0 mmol) dropwise. The resulting mixture was then refluxed for 3 h. After cooling, the reaction mixture was diluted with water and extracted with DCM. The combined organic layers were washed with brine and dried over anhydrous Na2SO4. After filtration and concentration, the crude product was purified by column chromatography to give the title compound (2.5 g, 88%).

후처리

  1. temperatureThe resulting mixture was then refluxed for 3 h
  2. temperatureAfter cooling
  3. extractionextracted with DCM
  4. washThe combined organic layers were washed with brine
  5. dry with materialdried over anhydrous Na2SO4
  6. filtrationAfter filtration and concentration
  7. customthe crude product was purified by column chromatography

출처 및 근거

ORD 기록
ord-8f2f7dadcfb54f70a3ac5351c3838360
출처 데이터셋
uspto-grants-2014_04
특허 번호
US08710245B2

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