1-(4-n-Hexyloxybenzoyl)-2-(4-methoxycarbonylbenzoyl)hydrazine → Aibmxqrtbasmnp-uhfffaoysa-

HRID 1386621노트

반응식

HRID 1386621 반응식
[CH2:1]([O:7][C:8]1[CH:29]=[CH:28][C:11]([C:12]([NH:14][NH:15][C:16](=O)[C:17]2[CH:22]=[CH:21][C:20]([C:23]([O:25][CH3:26])=[O:24])=[CH:19][CH:18]=2)=[O:13])=[CH:10][CH:9]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6]>P(Cl)(Cl)(Cl)=O>[CH2:1]([O:7][C:8]1[CH:9]=[CH:10][C:11]([C:12]2[O:13][C:16]([C:17]3[CH:18]=[CH:19][C:20]([C:23]([O:25][CH3:26])=[O:24])=[CH:21][CH:22]=3)=[N:15][N:14]=2)=[CH:28][CH:29]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH3:6]

참가 물질

3

반응물 1

HCID 171784121-(4-n-Hexyloxybenzoyl)-2-(4-methoxycarbonylbenzoyl)hydrazine

생성물 1

HCID 21182386Aibmxqrtbasmnp-uhfffaoysa-수율 79.7%

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

A suspension of 1-(4-n-Hexyloxybenzoyl)-2-(4-methoxycarbonylbenzoyl)hydrazine (1.00 g) in phosphorus oxychloride (5 ml) was refluxed for 1 hour. After cooling, the solution was concentrated under reduced pressure. The residue was poured into ice-water and extracted with dichloromethane. The organic layer was washed with water, brine and dried over magnesium sulfate. The solvents were removed under reduced pressure. The residue was triturated with acetonitrile, collected by filtration and dried under reduced pressure to give Methyl 4-[5-(4-n-hexyloxyphenyl)-1,3,4-oxadiazole-2-yl]benzoate (761 mg).

후처리

  1. temperaturewas refluxed for 1 hour
  2. temperatureAfter cooling
  3. concentrationthe solution was concentrated under reduced pressure
  4. additionThe residue was poured into ice-water
  5. extractionextracted with dichloromethane
  6. washThe organic layer was washed with water, brine
  7. dry with materialdried over magnesium sulfate
  8. customThe solvents were removed under reduced pressure
  9. customThe residue was triturated with acetonitrile
  10. filtrationcollected by filtration
  11. customdried under reduced pressure

출처 및 근거

ORD 기록
ord-49ae3ad4e9eb4c75b812efbcc949bec9
출처 데이터셋
uspto-grants-2001_07
특허 번호
US06265536B1

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