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

HRID 443851
ノート
印刷プレビュー

反応式

HRID 443851 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-c3775460aa7549e6b528de6502790255
出典データセット
uspto-grants-1981_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04261997

反応ノート

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