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Water → HCID 57736351, 화합물

HRID 2261331
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HRID 2261331 반응식
F[C:2](F)([C:8]([F:17])([F:16])[C:9]([F:15])([F:14])[C:10]([F:13])([F:12])[F:11])[CH:3]=[C:4](I)[CH2:5][OH:6].[OH2:19].Cl.[NH2:21]O.C(=O)([O-])[O-].[K+].[K+]>C(O)C>[F:14][C:9]([F:15])([C:10]([F:13])([F:12])[F:11])[C:8]([F:17])([F:16])[C:2]1[O:19][N:21]=[C:4]([CH2:5][OH:6])[CH:3]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 11430Potassium CarbonateHCID 443297Hydroxyamine hydrochlorideHCID 86631047HCID 86631047, 화합물

생성물 1

HCID 57736351HCID 57736351, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

14.94 g of 4,4,5,5,6,6,7,7,7-nonafluoro-2-iodo-2-heptene-1-ol was dissolved in 150 ml of ethanol, and 70 ml of water, 5.17 g of hydroxylamine hydrochloride and 25.67 g of potassium carbonate were then added. The mixture was stirred and heated under reflux for 24 hours. The reaction mixture was concentrated under reduced pressure. After water was added, the residue 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 3.53 g of (5-heptafluoropropyl-isoxazol-3-yl)methanol.

후처리

  1. temperatureheated
  2. temperatureunder reflux for 24 hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. additionAfter water was added
  5. extractionthe residue was extracted with ethyl acetate
  6. washThe organic layer was washed with water
  7. dry with materialdried over anhydrous magnesium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-608d1c8e3d7847f3bf2cdc3ddd200e19
출처 데이터셋
uspto-grants-2010_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07846956B2

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