Hydrogen Peroxide → 2-Carboxyphenoxathiin-10-oxide

HRID 372487

반응식

HRID 372487 반응식
[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]

참가 물질

4

반응물 2

HCID 784Hydrogen Peroxide2회HCID 8200622-Phenoxathiincarboxylic acid

생성물 1

HCID 203277292-Carboxyphenoxathiin-10-oxide

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-80a36d2874b643b1b071bb17972b06a1
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04091108

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