Sodium Hydroxide → HCID 1793644、化合物

HRID 1979721ノート

反応式

HRID 1979721 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9]1=[CH:15][C:16](Cl)=[N:17][C:18](=[O:19])[N:8]1[CH2:7][CH2:6]2.[OH-:21].[Na+]>C(O)CCC>[CH3:1][O:2][C:3]1[CH:4]=[C:5]2[C:10](=[CH:11][C:12]=1[O:13][CH3:14])[C:9]1=[CH:15][C:16]([O:21][CH2:4][CH2:3][CH2:12][CH3:11])=[N:17][C:18](=[O:19])[N:8]1[CH2:7][CH2:6]2

参加物

4

反応物 2

HCID 14798Sodium HydroxideHCID 46787202-Chloro-6,7-dihydro-9,10-dimethoxy-4H-pyrimido[6,1-a]isoquinolin-4-one

生成物 1

HCID 1793644HCID 1793644、化合物収率 85%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

1.46 g of 9,10-dimethoxy-6,7-dihydro-2-chloro-4H-pyrimido(6,1-a)isoquinolin-4-one are added to a mixture of 1.0 g of sodium hydroxide and 50.0 ml of n-butanol. The reduction mixture is refluxed for 6 hours. The solvent is removed under reduced pressure. The residue is treated with water and extracted with chloroform. The extract is dried over anhydrous Na2SO4 and evaporated to give a white solid. After crystallization from a chloroform-ether mixture, 0.7 g of the title compound is obtained, m.p. 158°-159° C.

後処理

  1. temperatureThe reduction mixture is refluxed for 6 hours
  2. customThe solvent is removed under reduced pressure
  3. additionThe residue is treated with water
  4. extractionextracted with chloroform
  5. dry with materialThe extract is dried over anhydrous Na2SO4
  6. customevaporated
  7. customto give a white solid
  8. customAfter crystallization from a chloroform-ether mixture

出典と根拠

ORDレコード
ord-52ec23814c77492cb17822f72233488a
出典データセット
uspto-grants-1984_11
特許番号
US04482556

反応ノート

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