Sodium Hydroxide → HCID 1793644, 화합물

HRID 1979721노트

반응식

HRID 1979721 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

HCID 1793644HCID 1793644, 화합물수율 85%

시약·촉매·용매 1

HCID 2631-Butanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-52ec23814c77492cb17822f72233488a
출처 데이터셋
uspto-grants-1984_11
특허 번호
US04482556

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