6-[4-(2-t-butoxycarbonylamino-2-methylpropylamino)phenyl]-5-methyl-4,5-dihydro-3(2H)-pyridazinone → 6-[4-(2-amino-2-methylpropyl amino)phenyl]-5-methyl-4,5-dihydro-3(2H)-pyridazinone

HRID 1905416ノート

反応式

HRID 1905416 の反応式
C(OC([NH:8][C:9]([CH3:27])([CH3:26])[CH2:10][NH:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]2[CH:19]([CH3:25])[CH2:20][C:21](=[O:24])[NH:22][N:23]=2)=[CH:14][CH:13]=1)=O)(C)(C)C.C(OCC)(=O)C.Cl>C(OCC)(=O)C>[NH2:8][C:9]([CH3:26])([CH3:27])[CH2:10][NH:11][C:12]1[CH:13]=[CH:14][C:15]([C:18]2[CH:19]([CH3:25])[CH2:20][C:21](=[O:24])[NH:22][N:23]=2)=[CH:16][CH:17]=1

参加物

4

反応物 2

HCID 108332506-[4-(2-t-butoxycarbonylamino-2-methylpropylamino)phenyl]-5-methyl-4,5-dihydro-3(2H)-pyridazinoneHCID 21866389Hydrogen chloride-ethyl acetate

生成物 1

HCID 106123876-[4-(2-amino-2-methylpropyl amino)phenyl]-5-methyl-4,5-dihydro-3(2H)-pyridazinone収率 75.2%

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

The 6-[4-(2-t-butoxycarbonylamino-2-methylpropylamino)phenyl]-5-methyl-4,5-dihydro-3(2H)-pyridazinone (3.74 g) obtained in (1-c) above was dissolved in ethyl acetate (10 ml), and 15% hydrogen chloride-ethyl acetate solution (40 ml) was added. The mixture was stirred for 2 hours, and the solvent was evaporated under reduced pressure. The residue was dissolved in water, made alkaline with sodium carbonate, and extracted with chloroform. The extract was dried over MgSO4, and the solvent was evaporated to give 6-[4-(2-amino-2-methylpropylamino)phenyl]-5-methyl-4,5-dihydro-3(2H)-pyridazinone (2.06 g).

後処理

  1. customthe solvent was evaporated under reduced pressure
  2. dissolutionThe residue was dissolved in water
  3. extractionextracted with chloroform
  4. dry with materialThe extract was dried over MgSO4
  5. customthe solvent was evaporated

出典と根拠

ORDレコード
ord-1da59c6e06b340ceb817b9d8b21d183b
出典データセット
uspto-grants-1989_06
特許番号
US04843072

反応ノート

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