Hydrogen Peroxide → 2-Carboxyphenoxathiin-10-oxide

HRID 372487

反応式

HRID 372487 の反応式
[CH:1]1[C:14]2[S:13][C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[O:6][C:5]=2[CH:4]=[CH:3][C:2]=1[C:15]([OH:17])=[O:16].[OH:18]O>C(O)C>[C:15]([C:2]1[CH:3]=[CH:4][C:5]2[O:6][C:7]3[C:12](=[CH:11][CH:10]=[CH:9][CH:8]=3)[S:13](=[O:18])[C:14]=2[CH:1]=1)([OH:17])=[O:16]

参加物

4

反応物 2

HCID 784Hydrogen Peroxide2 回HCID 8200622-Phenoxathiincarboxylic acid

生成物 1

HCID 203277292-Carboxyphenoxathiin-10-oxide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Phenoxathiin-2-carboxylic acid (0.61g) was dissolved in refluxing absolute ethanol (40 ml) and 30% w/v hydrogen peroxide solution (1.50 ml) added. Reflux was maintained for 2 hours, more 30% w/v hydrogen peroxide solution (1.00 ml.) added, and reflux continued for 17 hours. The solution was evaporated to low volume, and the product crystallised out. The solid was filtered, washed and dried to give 2-carboxyphenoxathiin-10-oxide m.p. 223° C. Recrystallisation from absolute ethanol raised the melting point to 237° C.

後処理

  1. additionadded
  2. temperatureReflux
  3. temperaturewas maintained for 2 hours
  4. additionadded
  5. temperaturereflux
  6. customThe solution was evaporated to low volume
  7. customthe product crystallised out
  8. filtrationThe solid was filtered
  9. washwashed
  10. customdried

出典と根拠

ORDレコード
ord-80a36d2874b643b1b071bb17972b06a1
出典データセット
uspto-grants-1978_05
特許番号
US04091108

関連ノート

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