Hydrazine → bemoradan

HRID 1588334ノート

反応式

HRID 1588334 の反応式
[O:1]=[C:2]1[NH:7][C:6]2[CH:8]=[CH:9][C:10]([C:12](=O)[CH:13]([CH3:18])[CH2:14][C:15](O)=[O:16])=[CH:11][C:5]=2[O:4][CH2:3]1.[NH2:20][NH2:21]>C(O)C>[O:1]=[C:2]1[NH:7][C:6]2[CH:8]=[CH:9][C:10]([C:12]3[CH:13]([CH3:18])[CH2:14][C:15](=[O:16])[NH:20][N:21]=3)=[CH:11][C:5]=2[O:4][CH2:3]1

参加物

4

反応物 2

HCID 9321HydrazineHCID 11065271HCID 11065271、化合物

生成物 1

HCID 5362399bemoradan収率 93%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

4-(3,4-Dihydro-3-oxo-1,4(2H)-benzoxazin-7-yl)-4-oxo-3-methylbutyric acid (31 g, 0.12 moles) was dissolved in ethanol (300 ml) and anhydrous hydrazine (4.7 ml, 0.15 moles) was added. The mixture was heated at reflux overnight. White crystals formed after the mixture was cooled. The crystals were collected by filtration and washed well with ethanol. The solid was dried under vacuum giving 28.5 g (93%) of the titled compound, mp 299°-302° C.

後処理

  1. temperatureThe mixture was heated
  2. temperatureat reflux overnight
  3. customWhite crystals formed after the mixture
  4. temperaturewas cooled
  5. filtrationThe crystals were collected by filtration
  6. washwashed well with ethanol
  7. customThe solid was dried under vacuum

出典と根拠

ORDレコード
ord-9ab5686fe7e246cc8b97ed1e68459d7b
出典データセット
uspto-grants-1993_06
特許番号
US05221742

反応ノート

読み込み中…