Benzoic Acid → 2-phenyl-1,3-benzoxazol-5-amine

HRID 1896738

반응식

HRID 1896738 반응식
Cl.Cl.[NH2:3][C:4]1[CH:9]=[C:8]([NH2:10])[CH:7]=[CH:6][C:5]=1[OH:11].[C:12](O)(=O)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1>O>[C:13]1([C:12]2[O:11][C:5]3[CH:6]=[CH:7][C:8]([NH2:10])=[CH:9][C:4]=3[N:3]=2)[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1

참가 물질

4

반응물 2

HCID 243Benzoic AcidHCID 87152,4-Diaminophenol hydrochloride

생성물 1

HCID 7210592-phenyl-1,3-benzoxazol-5-amine수율 97%

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
180 °C

실험 절차

To polyphosphoric acid at 110° C. were added simultaneously 2,4-diaminophenol dihydrochloride (7.88 g, 40 mmol) and benzoic acid (4.88 g, 40 mmol). The resulting mixture was then heated to 180° C. for 3 h. The solution was then poured into water. The resulting precipitate was collected by filtration and washed with saturated sodium bicarbonate solution. The crude product was recrystallised from ethanol/water to afford 8.15 g (97%) of the title compound (LCMS RT=5.17 min, MH+ 211.1)

후처리

  1. filtrationThe resulting precipitate was collected by filtration
  2. washwashed with saturated sodium bicarbonate solution
  3. customThe crude product was recrystallised from ethanol/water

출처 및 근거

ORD 기록
ord-6b8a684af1a24d0a815520d09caf1cfb
출처 데이터셋
uspto-grants-2013_08
특허 번호
US08518980B2

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