Chloroform → HCID 23145779, 화합물

HRID 13348

반응식

HRID 13348 반응식
C(Cl)(Cl)Cl.[N+:5]([C:8]1[CH:15]=[CH:14][C:11]([CH:12]=[O:13])=[C:10]([F:16])[CH:9]=1)([O-:7])=[O:6].[CH2:17]([Si](C)(C)C)[CH:18]=[CH2:19]>C(OCC)(=O)C.[Ti](Cl)(Cl)(Cl)Cl>[F:16][C:10]1[CH:9]=[C:8]([N+:5]([O-:7])=[O:6])[CH:15]=[CH:14][C:11]=1[CH:12]([OH:13])[CH2:19][CH:18]=[CH2:17]

참가 물질

6

반응물 3

HCID 6212ChloroformHCID 69808AllyltrimethylsilaneHCID 45629192-Fluoro-4-nitrobenzaldehyde

생성물 1

HCID 23145779HCID 23145779, 화합물

시약·촉매·용매 2

HCID 24193Titanium Tetrachloride촉매HCID 8857Ethyl Acetate용매

실험 절차

0.65 ml of titanium tetrachloride was added to a chloroform (12 ml) solution of 2.00 g of 4-nitro-2-fluoro-benzaldehyde produced according to the method described in U.S. Pat. No. 6,239,152, and the reaction liquid was stirred at room temperature for 10 minutes, and then 2.4 ml of allyl-trimethyl-silane was added to it, and the reaction liquid was stirred at room temperature for 20 minutes. The reaction liquid was diluted with ethyl acetate, washed with water and saturated saline, and dried with anhydrous sodium sulfate. The solvent was evaporated away under reduced pressure, and the residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=3/1) to obtain the entitled compound as an orange solid.

후처리

  1. customproduced
  2. custom6,239,152, and the reaction liquid
  3. customthe reaction liquid
  4. stirringwas stirred at room temperature for 20 minutes
  5. customThe reaction liquid
  6. washwashed with water and saturated saline
  7. dry with materialdried with anhydrous sodium sulfate
  8. customThe solvent was evaporated away under reduced pressure
  9. customthe residue was purified through silica gel column chromatography (developing solvent: hexane/ethyl acetate=3/1)

출처 및 근거

ORD 기록
ord-e409d2c505314342bc35b68cf061a516
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07728025B2

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