Chloroform → HCID 23145779、化合物

HRID 13348

反応式

HRID 13348 の反応式
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]

参加物

6

反応物 3

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

生成物 1

HCID 23145779HCID 23145779、化合物

試薬・触媒・溶媒 2

HCID 24193Titanium Tetrachloride触媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-e409d2c505314342bc35b68cf061a516
出典データセット
uspto-grants-2010_06
特許番号
US07728025B2

関連ノート

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