Hydroxyamine hydrochloride → 5-(2,4-Dichloro-5-fluorophenyl)-isoxazole

HRID 2118792

반응식

HRID 2118792 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([F:9])=[CH:4][C:3]=1[C:10]([CH:12]=[CH:13]Cl)=[O:11].Cl.[NH2:16]O>CO>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([F:9])=[CH:4][C:3]=1[C:10]1[O:11][N:16]=[CH:13][CH:12]=1

참가 물질

4

반응물 2

HCID 443297Hydroxyamine hydrochlorideHCID 542986662-Chlorovinyl 2,4-dichloro5-fluoro-phenyl ketone

생성물 1

HCID 136307205-(2,4-Dichloro-5-fluorophenyl)-isoxazole

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 57.6 g of 2-chlorovinyl 2,4-dichloro-5-fluoro-phenyl ketone, 16.4 g of hydroxylamine hydrochloride and 150 ml of methanol is heated at the boiling point under reflux for 6 hours, a precipitate separating out after about one hour. This is filtered off cold with suction, washed with a little methanol and dried at 50° C. in vacuo. 33.3 g (63.2%) of 5-(2,4-dichloro-5-fluorophenyl)-isoxazole of melting point 112°-113° C., which, according to investigations by NMR spectroscopy, contains about 6 mole % of an isomer, are obtained.

후처리

  1. temperatureis heated at the boiling point
  2. temperatureunder reflux for 6 hours
  3. customa precipitate separating out after about one hour
  4. filtrationThis is filtered off cold with suction
  5. washwashed with a little methanol
  6. customdried at 50° C. in vacuo
  7. customare obtained

출처 및 근거

ORD 기록
ord-76afefc6c87b401aa7b16eb766e39b5d
출처 데이터셋
uspto-grants-1987_07
특허 번호
US04680401

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