HCID 10757175、化合物 → HCID 18687725、化合物

HRID 1872880ノート

反応式

HRID 1872880 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[S:6](=[O:21])(=[O:20])[C:7]3[C:12]([O:13][C:14]=2[CH:15]=1)=[CH:11][C:10]([O:16]C(C)C)=[CH:9][CH:8]=3>S([O-])(O)(=O)=O.C([N+](CCCC)(CCCC)CCCC)CCC.Br>[F:1][C:2]1[CH:3]=[CH:4][C:5]2[S:6](=[O:21])(=[O:20])[C:7]3[C:12]([O:13][C:14]=2[CH:15]=1)=[CH:11][C:10]([OH:16])=[CH:9][CH:8]=3

参加物

4

反応物 1

HCID 10757175HCID 10757175、化合物

生成物 1

HCID 18687725HCID 18687725、化合物収率 99.3%

試薬・触媒・溶媒 2

HCID 94433Tetrabutylammonium hydrogen sulfate触媒HCID 260Hydrogen Bromide溶媒

実験手順

A mixture of 3-fluoro-7-isopropoxyphenoxathiin 10,10-dioxide (Example 9) (3.51 g, 11.39 mmoles), tetrabutylammonium hydrogen sulfate (Aldrich) (0.654 g, 1.93 mmoles) and 48% aqueous hydrogen bromide (Acros) (80 mL) was refluxed with stirring for 45 minutes. The reaction was allowed to cool on an ice-bath, and the solid was collected, washed with water and dried in vacuo to give 3.010 g (99%) of 3-fluoro-7-hydroxyphenoxathiin 10,10-dioxide, mp 258-260° C. Recrystallization from ethyl acetate:hexanes gave the analytical sample, m.p. 250-260° C.

後処理

  1. temperaturewas refluxed
  2. temperatureto cool on an ice-bath
  3. customthe solid was collected
  4. washwashed with water
  5. customdried in vacuo

出典と根拠

ORDレコード
ord-ef965f9c495f4cd8be389c9044e066fc
出典データセット
uspto-grants-2000_08
特許番号
US06110961

反応ノート

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