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

HRID 1250596노트

반응식

HRID 1250596 반응식
[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]

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-1b2d28acb524461e8e251cfc2ddcc283
출처 데이터셋
uspto-grants-2002_01
특허 번호
US06339089B2

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