Acetic Acid → 5-Methyl-3-phenyl-2,1-benzisoxazole

HRID 1198980노트

반응식

HRID 1198980 반응식
[CH3:1][C:2]1[CH:3]=[CH:4][C:5]([NH2:16])=[C:6]([CH:15]=1)[C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)=[O:8].C(O)(=O)C.OO>O>[CH3:1][C:2]1[CH:3]=[CH:4][C:5]2[C:6]([CH:15]=1)=[C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[O:8][N:16]=2

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 784Hydrogen PeroxideHCID 873352-Amino-5-methylbenzophenone

생성물 1

HCID 6106335-Methyl-3-phenyl-2,1-benzisoxazole

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 31.6 g (0.15 mole) of 5-methyl-2-aminobenzophenone, 350 ml of glacial acetic acid and 17 ml of 30% hydrogen peroxide was let stand at ambient temperature for 72 hr. The solution was poured into 2.5 liters of water. The mixture was let stand at ambient temperature for several days until the residue became crystalline. The solid was collected by filtration, dried, and chromatographed on 250 g silica gel to give 12.5 g (40%) of pale yellow solid, m.p. 64°-66° C. (after recrystallization from 2-propanol).

후처리

  1. customat ambient temperature
  2. customfor several days
  3. filtrationThe solid was collected by filtration
  4. customdried
  5. customchromatographed on 250 g silica gel
  6. customto give
  7. custom12.5 g (40%) of pale yellow solid, m.p. 64°-66° C. (after recrystallization from 2-propanol)

출처 및 근거

ORD 기록
ord-20740d0113b34d2cb3f23e4fdf7a12ed
출처 데이터셋
uspto-grants-1990_02
특허 번호
US04898874

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