Sodium Chloride → HCID 22042477、化合物

HRID 1790886ノート

反応式

HRID 1790886 の反応式
[Cl-].[Li+].COP([CH2:9][CH2:10][CH:11]=[O:12])(=O)OC.[CH:13](N(C(C)C)CC)(C)C.[CH3:22][C:23]1([C:28]2(C=O)[CH2:30][CH2:29]2)[O:27][CH2:26][CH2:25][O:24]1.[Cl-].[Na+]>C(#N)C>[CH3:22][C:23]1([C:28]2(/[CH:9]=[CH:10]/[C:11](=[O:12])[CH3:13])[CH2:30][CH2:29]2)[O:27][CH2:26][CH2:25][O:24]1

参加物

7

反応物 5

HCID 5234Sodium ChlorideHCID 81531DiisopropylethylamineHCID 433294Lithium ChlorideHCID 11147922oxopropylphosphonic acid dimethyl esterHCID 143755571-(2-Methyl-1,3-dioxolan-2-YL)cyclopropane-1-carbaldehyde

生成物 1

HCID 22042477HCID 22042477、化合物

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

13.8 g of lithium chloride (anhydrous) is introduced into 120 ml of acetonitrile under nitrogen, and 49.8 ml of oxopropylphosphonic acid dimethyl ester, 51.3 ml of diisopropylethylamine and 5.4 g of aldehyde 7 are added in succession. It is stirred for 18 hours at room temperature, and then sodium chloride solution is added. It is extracted with ethyl acetate, washed with sodium chloride solution and dried on sodium sulfate. The residue is chromatographed on silica gel with ethyl acetate/hexane, whereby 5.3 g of the title compound accumulates as a colorless oil.

後処理

  1. extractionIt is extracted with ethyl acetate
  2. washwashed with sodium chloride solution
  3. customdried on sodium sulfate
  4. customThe residue is chromatographed on silica gel with ethyl acetate/hexane, whereby 5.3 g of the title compound accumulates as a colorless oil

出典と根拠

ORDレコード
ord-f5acf844c5c24b999fc9ae28f72b4c88
出典データセット
uspto-grants-2006_07
特許番号
US07071344B1

反応ノート

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