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

HRID 1198980ノート

反応式

HRID 1198980 の反応式
[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

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-20740d0113b34d2cb3f23e4fdf7a12ed
出典データセット
uspto-grants-1990_02
特許番号
US04898874

反応ノート

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