Chloroform → HCID 18689381, 화합물

HRID 1871846

반응식

HRID 1871846 반응식
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

참가 물질

6

반응물 5

HCID 6212Chloroform2회HCID 7912DiisopropylamineHCID 32745N-Chloro-N,N-diisopropylamineHCID 873033-Ketocarbofuran phenolHCID 23665760Sodium Hypochlorite

생성물 1

HCID 18689381HCID 18689381, 화합물

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-3716ee726c354d14860f7b291bc859a9
출처 데이터셋
uspto-grants-2000_08
특허 번호
US06107036

연결된 노트

불러오는 중…