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

HRID 1386621ノート

反応式

HRID 1386621 の反応式
[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]

参加物

3

反応物 1

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

生成物 1

HCID 21182386Aibmxqrtbasmnp-uhfffaoysa-収率 79.7%

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-49ae3ad4e9eb4c75b812efbcc949bec9
出典データセット
uspto-grants-2001_07
特許番号
US06265536B1

反応ノート

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