Chloroform → HCID 18689381、化合物

HRID 1871846

反応式

HRID 1871846 の反応式
O[C:2]1[C:10]2[O:9][C:8]([CH3:12])([CH3:11])[C:7](=[O:13])[C:6]=2[CH:5]=[CH:4]C=1.ClN(C(C)C)C(C)C.C(NC(C)C)(C)C.Cl[O-:30].[Na+].[CH:32]([Cl:35])(Cl)Cl>>[Cl:35][C:32]1[C:4]([OH:30])=[CH:5][C:6]2[C:7](=[O:13])[C:8]([CH3:12])([CH3:11])[O:9][C:10]=2[CH:2]=1

参加物

6

反応物 5

HCID 6212Chloroform2 回HCID 7912DiisopropylamineHCID 32745N-Chloro-N,N-diisopropylamineHCID 873033-Ketocarbofuran phenolHCID 23665760Sodium Hypochlorite

生成物 1

HCID 18689381HCID 18689381、化合物

実験手順

25 mmol 7-Hydroxy-2,2-dimethyl-benzofuran-3-one and 30 g silica gel are stirred in 200 ml chloroform. A solution of 25 mmol N-chloro-diisopropylamine in 100 ml chloroform (prepared from diisopropylamine and aqueous sodium hypochlorite solution, extracted in chloroform, concentration determined iodometrically) is added dropwise. After stirring for 10 hours it is filtered and the filtrate is shaken out with water. The solution is dried over sodium sulfate. The solvent is removed by distillation at 300 mbar. The residue is separated by column chromatography (silica gel: ethyl acetate).

後処理

  1. extractionextracted in chloroform
  2. concentrationconcentration determined iodometrically)
  3. additionis added dropwise
  4. filtrationis filtered
  5. stirringthe filtrate is shaken out with water
  6. dry with materialThe solution is dried over sodium sulfate
  7. customThe solvent is removed by distillation at 300 mbar
  8. customThe residue is separated by column chromatography (silica gel: ethyl acetate)

出典と根拠

ORDレコード
ord-3716ee726c354d14860f7b291bc859a9
出典データセット
uspto-grants-2000_08
特許番号
US06107036

関連ノート

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