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Sodium Hydroxide → 4,9-Dihydro-4-methyl-9-oxo-pyrazolo[5,1-b]quinazoline-2-carboxylic Acid

HRID 443851
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HRID 443851 반응식
[CH3:1][N:2]1[C:11]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[C:5](=[O:12])[N:4]2[N:13]=[C:14]([C:16]([O:18]CC)=[O:17])[CH:15]=[C:3]12.[OH-].[Na+]>CO>[CH3:1][N:2]1[C:11]2[CH:10]=[CH:9][CH:8]=[CH:7][C:6]=2[C:5](=[O:12])[N:4]2[N:13]=[C:14]([C:16]([OH:18])=[O:17])[CH:15]=[C:3]12
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 125525054,9-Dihydro-4-methyl-9-oxo-pyrazolo[5,1-b]quinazoline-2-carboxylic acid, ethyl ester

생성물 1

HCID 127132494,9-Dihydro-4-methyl-9-oxo-pyrazolo[5,1-b]quinazoline-2-carboxylic Acid

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A mixture of 5.8 g of 4,9-dihydro-4-methyl-9-oxo-pyrazolo[5,1-b]quinazoline-2-carboxylic acid, ethyl ester, 50 ml of 1 N aqueous sodium hydroxide and 400 ml of methanol is heated at reflux until complete solution is attained (about 30 minutes). The solution is evaporated at reduced pressure to remove methanol; the residue is diluted with water and acidified with 1 N hydrochloric acid. The resulting precipitate is 4,9-dihydro-4-methyl-9-oxo-pyrazolo[5,1-b]quinazoline-2-carboxylic acid is collected by filtration, washed with water and dried; mp 265° C., after crystallization from dimethylformamide/methanol.

후처리

  1. temperatureis heated
  2. temperatureat reflux until complete solution
  3. custom(about 30 minutes)
  4. customThe solution is evaporated at reduced pressure
  5. customto remove methanol
  6. additionthe residue is diluted with water
  7. filtrationis collected by filtration
  8. washwashed with water
  9. customdried
  10. custommp 265° C., after crystallization from dimethylformamide/methanol

출처 및 근거

ORD 기록
ord-c3775460aa7549e6b528de6502790255
출처 데이터셋
uspto-grants-1981_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04261997

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