Hydrazine → HCID 178518904, 화합물

HRID 2357513노트

반응식

HRID 2357513 반응식
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

참가 물질

4

반응물 2

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

생성물 1

HCID 178518904HCID 178518904, 화합물수율 98.6%

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

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.).

후처리

  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

출처 및 근거

ORD 기록
ord-1cc79bce83f54b89a8aef1d1ae90c871
출처 데이터셋
uspto-grants-2010_07
특허 번호
US07759337B2

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