Hydrazine → HCID 178518904、化合物

HRID 2357513ノート

反応式

HRID 2357513 の反応式
C([N:5]1[CH:13](O)[C:12]2[C:7](=[CH:8][CH:9]=[C:10]([Cl:15])[CH:11]=2)[C:6]1=[O:16])(C)(C)C.[NH2:17]N>C(O)(=O)C>[Cl:15][C:10]1[CH:11]=[C:12]2[C:7](=[CH:8][CH:9]=1)[C:6]([OH:16])=[N:17][N:5]=[CH:13]2

参加物

4

反応物 2

HCID 9321HydrazineHCID 251930612-Tert-butyl-5-chloro-3-hydroxyisoindolin-1-one

生成物 1

HCID 178518904HCID 178518904、化合物収率 98.6%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

A suspension of 2-tert-butyl-5-chloro-3-hydroxyisoindolin-1-one (5.26 g, 21.9 mmol) in glacial acetic acid (32 mL) was heated with stirring until the mixture became a clear solution. Anhydrous hydrazine (1.0 mL, 22 mmol) was added dropwise and the resultant solution was stirred at reflux overnight. The reaction mixture was concentrated under reduced pressure. Water was added to the mixture, after which a solid material precipitated out of the solution. The solid was collected by filtration and rinsed thoroughly with water, followed by air-drying to afford 6-chlorophthalazin-1-ol (3.9 g, 98% yield) as an off-white powder (mp 271-273° C.).

後処理

  1. temperaturewas heated
  2. temperatureat reflux overnight
  3. concentrationThe reaction mixture was concentrated under reduced pressure
  4. additionWater was added to the mixture
  5. customafter which a solid material precipitated out of the solution
  6. filtrationThe solid was collected by filtration
  7. washrinsed thoroughly with water
  8. customby air-drying

出典と根拠

ORDレコード
ord-1cc79bce83f54b89a8aef1d1ae90c871
出典データセット
uspto-grants-2010_07
特許番号
US07759337B2

反応ノート

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