Acetic Acid → 7-(4-Chlorophenyl)-8-isopropyl-2-methyl-3H-chromeno[7,8-d]imidazol-6-one

HRID 14491

반응식

HRID 14491 반응식
[NH2:1][C:2]1[C:11]([NH2:12])=[C:10]2[C:5]([C:6](=[O:23])[C:7]([C:16]3[CH:21]=[CH:20][C:19]([Cl:22])=[CH:18][CH:17]=3)=[C:8]([CH:13]([CH3:15])[CH3:14])[O:9]2)=[CH:4][CH:3]=1.Cl.[C:25](O)(=O)[CH3:26]>C(OCC)(=O)C>[Cl:22][C:19]1[CH:18]=[CH:17][C:16]([C:7]2[C:6](=[O:23])[C:5]3[CH:4]=[CH:3][C:2]4[NH:1][C:25]([CH3:26])=[N:12][C:11]=4[C:10]=3[O:9][C:8]=2[CH:13]([CH3:14])[CH3:15])=[CH:21][CH:20]=1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 313Hydrochloric AcidHCID 687024427,8-Diamino-3-(4-chlorophenyl)-2-isopropyl-chromen-4-one

생성물 1

HCID 687002777-(4-Chlorophenyl)-8-isopropyl-2-methyl-3H-chromeno[7,8-d]imidazol-6-one

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

반응 조건

온도
120 °C

실험 절차

7,8-Diamino-3-(4-chlorophenyl)-2-isopropyl-chromen-4-one (80 mg, 0.243 mmol) is dissolved in glacial acetic acid (1.5 ml), dilute hydrochloric acid (2M, 0.1 ml) is added, and the mixture is heated at 120° C. for 90 min. The reaction mixture is cooled to room temperature, diluted with ethyl acetate (50 ml) and washed with saturated sodium bicarbonate solution (3×40 ml), water (40 ml) and saturated brine (40 ml). The organic layer is dried (MgSO4), filtered and evaporated to give a brown solid. This is triturated with ethyl acetate containing a few drops of methanol and filtered to give a pale yellow powder.

후처리

  1. temperatureThe reaction mixture is cooled to room temperature
  2. washwashed with saturated sodium bicarbonate solution (3×40 ml), water (40 ml) and saturated brine (40 ml)
  3. dry with materialThe organic layer is dried (MgSO4)
  4. filtrationfiltered
  5. customevaporated
  6. customto give a brown solid
  7. customThis is triturated with ethyl acetate containing a few drops of methanol
  8. filtrationfiltered
  9. customto give a pale yellow powder

출처 및 근거

ORD 기록
ord-179dcdbfab8a424ba6bff2c4a2d93f6e
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07732435B2

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