Water → 4-Allylamino-6-nitro-2-(propylcarbamoyl)aminoquinazoline

HRID 1250596ノート

反応式

HRID 1250596 の反応式
[CH2:1]([NH:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([N+:15]([O-:17])=[O:16])[CH:13]=2)[N:8]=[C:7]([NH2:18])[N:6]=1)[CH:2]=[CH2:3].[CH2:19]([N:22]=[C:23]=[O:24])[CH2:20][CH3:21].C(N(CC)CC)C.O>C1COCC1>[CH2:1]([NH:4][C:5]1[C:14]2[C:9](=[CH:10][CH:11]=[C:12]([N+:15]([O-:17])=[O:16])[CH:13]=2)[N:8]=[C:7]([NH:18][C:23](=[O:24])[NH:22][CH2:19][CH2:20][CH3:21])[N:6]=1)[CH:2]=[CH2:3]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 61033Propyl isocyanateHCID 183264494-Allylamino-2-amino-6-nitroquinazoline

生成物 1

HCID 183264484-Allylamino-6-nitro-2-(propylcarbamoyl)aminoquinazoline収率 80.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

After 200 mg (0.82 mmol) of 4-allylamino-2-amino-6-nitroquinazoline was dissolved in 10 ml of THF, 153 mg (1.80 mmol) of propylisocyanate and 0.13 ml (0.90 mmol) of triethylamine were added thereto, and then the reaction mixture was subjected to heating under reflux overnight. Water was added to the reaction solution, followed by extraction with ethyl acetate, washing with brine and drying over anhydrous sodium sulfate. After the solvent was distilled off, the residue was purified by a silica gel column to give 218 mg (80.5%) of the title compound.

後処理

  1. temperatureto heating
  2. temperatureunder reflux overnight
  3. extractionfollowed by extraction with ethyl acetate
  4. washwashing with brine
  5. dry with materialdrying over anhydrous sodium sulfate
  6. distillationAfter the solvent was distilled off
  7. customthe residue was purified by a silica gel column

出典と根拠

ORDレコード
ord-1b2d28acb524461e8e251cfc2ddcc283
出典データセット
uspto-grants-2002_01
特許番号
US06339089B2

反応ノート

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