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Water → HCID 57736344, 화합물

HRID 2261343
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HRID 2261343 반응식
[Si:1]([O:8][CH2:9][C:10]1[O:14][N:13]=[C:12]([CH2:15]O)[CH:11]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].C1(C)C=CC(S([Cl:26])(=O)=O)=CC=1.O>N1C=CC=CC=1>[Si:1]([O:8][CH2:9][C:10]1[O:14][N:13]=[C:12]([CH2:15][Cl:26])[CH:11]=1)([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 73974-Toluenesulfonyl chlorideHCID 57736305HCID 57736305, 화합물

생성물 1

HCID 57736344HCID 57736344, 화합물수율 22.3%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

18.64 g of [5-(t-butyldimethylsilanyloxymethyl)isoxazol-3-yl]methanol was dissolved in 80 ml of pyridine, and 16.06 g of 4-toluenesulfonyl chloride was then added under ice-cooling. The mixture was stirred for 10 hours under ice-cooling. After water was added, the reaction mixture was extracted with ethyl acetate. The organic layer was washed with water, dried over anhydrous magnesium sulfate, filtered and then concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to obtain 4.48 g of 5-(t-butyldimethylsilanyloxymethyl)-3-(chloromethyl)isoxazole.

후처리

  1. temperaturecooling
  2. temperaturecooling
  3. extractionthe reaction mixture was extracted with ethyl acetate
  4. washThe organic layer was washed with water
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-aa45def689254ac089ae2d2403d9368d
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07846956B2

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