Water → HCID 66618821, 화합물

HRID 406356

반응식

HRID 406356 반응식
[F:1][C:2]([F:13])([F:12])[C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][C:4]=1[CH2:9][C:10]#[N:11].[OH-].[Na+].Br[CH2:17][CH2:18][O:19][Si:20]([C:23]([CH3:26])([CH3:25])[CH3:24])([CH3:22])[CH3:21].O>S(=O)(=O)(O)[O-].C([N+](CCCC)(CCCC)CCCC)CCC.C1(C)C=CC=CC=1>[Si:20]([O:19][CH2:18][CH2:17][CH:9]([C:4]1[CH:5]=[CH:6][CH:7]=[CH:8][C:3]=1[C:2]([F:12])([F:13])[F:1])[C:10]#[N:11])([C:23]([CH3:26])([CH3:25])[CH3:24])([CH3:22])[CH3:21]

참가 물질

7

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 764352-(Trifluoromethyl)phenylacetonitrileHCID 3608067(2-Bromoethoxy)-tert-butyldimethylsilane

생성물 1

HCID 66618821HCID 66618821, 화합물

시약·촉매·용매 2

HCID 94433Tetrabutylammonium hydrogen sulfate촉매HCID 1140Toluene용매

실험 절차

(2-Trifluoromethylphenyl)acetonitrile (3 g) and tetrabutylammonium bisulfate (550 mg) were suspended in toluene (30 mL), and a 50% sodium hydroxide aqueous solution (15 mL) was added dropwise under ice-cooling. After stirring for 10 minutes, (2-bromoethoxy)-tert-butyldimethylsilane (5.2 mL) was added at the same temperature. The mixture was brought back to room temperature and stirred overnight. Water was added to the reaction solution, followed by extraction with tert-butyl methyl ether. The resulting organic layer was washed with brine and then dried over anhydrous sodium sulfate. The drying agent was separated by filtration, and then the organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography to obtain the title compound (5 g). The property values of the compound are as follows.

후처리

  1. temperaturecooling
  2. customwas brought back to room temperature
  3. stirringstirred overnight
  4. extractionfollowed by extraction with tert-butyl methyl ether
  5. washThe resulting organic layer was washed with brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe drying agent was separated by filtration
  8. concentrationthe organic layer was concentrated under reduced pressure
  9. customThe residue was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-14290ab3a76e4b4499edd07543d5ccbe
출처 데이터셋
uspto-grants-2014_06
특허 번호
US08754100B2

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