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Methanol → Methyl 2-[3-(3-trifluoromethylphenyl)-5-isoxazolyl]benzoate

HRID 1706773
ノート
印刷プレビュー

反応式

HRID 1706773 の反応式
[F:1][C:2]([F:24])([F:23])[C:3]1[CH:4]=[C:5]([C:9]2[CH2:13][C:12]3([C:21]4[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=4)[C:15](=[O:22])[O:14]3)[O:11][N:10]=2)[CH:6]=[CH:7][CH:8]=1.S(=O)(=O)(O)O.[CH3:30]O>>[F:23][C:2]([F:24])([F:1])[C:3]1[CH:4]=[C:5]([C:9]2[CH:13]=[C:12]([C:21]3[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=3[C:15]([O:14][CH3:30])=[O:22])[O:11][N:10]=2)[CH:6]=[CH:7][CH:8]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 887MethanolHCID 1118Sulfuric AcidHCID 13071263HCID 13071263、化合物

生成物 1

HCID 13018699Methyl 2-[3-(3-trifluoromethylphenyl)-5-isoxazolyl]benzoate

実験手順

A mixture of 2 g. (0.006 mole) of 3'-(m-trifluoromethylphenyl)-spiro[isobenzofuran-1(3H), 5'(4'H)-isoxazol]-3-one, 2 ml. of concentrated sulfuric acid and 50 ml. of methanol was heated at reflux for 17 hours. The solution was then poured into 100 g. of ice and extracted twice with 300 ml. of ether. The ether solutions were combined, washed twice with water saturated sodium chloride, and dried over CaSO4. Removal of the solvent gave 2 g. of colorless viscous liquid, which was crystallized from hexane at 0° C. to give colorless crystals; m.p. 46°-48° C.

後処理

  • additionA mixture of 2 g
  • temperatureat reflux for 17 hours
  • additionThe solution was then poured into 100 g
  • extractionof ice and extracted twice with 300 ml
  • washwashed twice with water saturated sodium chloride
  • dry with materialdried over CaSO4
  • customRemoval of the solvent
  • customgave 2 g
  • customof colorless viscous liquid, which was crystallized from hexane at 0° C.
  • customto give colorless crystals
  • 出典と根拠

    ORDレコード
    ord-749f7d7c5fc241ab9cb0caf4bf341adf
    出典データセット
    uspto-grants-1980_06
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US04208510

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