Boron trifluoride etherate → HCID 20324958、化合物

HRID 838849ノート

反応式

HRID 838849 の反応式
[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]2[N:9]=[CH:10][CH:11]=[C:4]2[N:3]=1.[F:12]C(F)(F)C(OC(=O)C(F)(F)F)=O.B(F)(F)F.CCOCC.[OH-].[Na+]>C(Cl)Cl>[CH3:1][C:2]1[CH:7]=[C:6]([CH3:8])[N:5]2[N:9]=[CH:10][C:11]([F:12])=[C:4]2[N:3]=1

参加物

6

反応物 4

HCID 8000Boron trifluoride etherateHCID 9845Trifluoroacetic anhydrideHCID 14798Sodium HydroxideHCID 215186Pyrazolo(1,5-a)pyrimidine, 5,7-dimethyl-

生成物 1

HCID 20324958HCID 20324958、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 5,7-dimethyl pyrazolo[1,5-a]pyrimidine [1.47g (10 mmoles)], trifluoroacetic anhydride (2.0 ml), and boron trifluoride etherate (2.0 ml) in CH2Cl2 (30 ml) was heated at reflux for 24 hours. At the end of this time the red solution was cooled and added to an ice cold solution of NaOH (30 ml, 2N). The organic layer was separated and the alkaline layer extracted with CH2Cl2 3(20 ml). The combined CH2Cl2 extracts were washed with water 2(20 ml) and dried over Na2SO4. The CH2Cl2 extract was evaporated and the residue covered with n-petane qnd chilled. The yellow white crystalline plates were separated by filtration, and recrystallized from n-heptane to yield an analytically pure product; mp 129°-30°.

後処理

  1. temperaturewas heated
  2. temperatureat reflux for 24 hours
  3. temperatureAt the end of this time the red solution was cooled
  4. customThe organic layer was separated
  5. extractionthe alkaline layer extracted with CH2Cl2 3(20 ml)
  6. washThe combined CH2Cl2 extracts were washed with water 2(20 ml)
  7. dry with materialdried over Na2SO4
  8. extractionThe CH2Cl2 extract
  9. customwas evaporated
  10. temperaturechilled
  11. customThe yellow white crystalline plates were separated by filtration
  12. customrecrystallized from n-heptane
  13. customto yield an analytically pure product

出典と根拠

ORDレコード
ord-d49db4e2d9f44d74a2159c23710bdeda
出典データセット
uspto-grants-1978_06
特許番号
US04093617

反応ノート

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