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Hydrochloric Acid → 10,10-Dioxo-9,10-dihydro-10lambda~6~-thioxanthene-3-carboxylic acid

HRID 1447566
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HRID 1447566 반응식
[C:1]([C:4]1[CH:5]=[CH:6][C:7]2[C:8](=O)[C:9]3[C:14]([S:15](=[O:19])(=[O:18])[C:16]=2[CH:17]=1)=[CH:13][CH:12]=[CH:11][CH:10]=3)([OH:3])=[O:2].Cl>C(O)(=O)C.[Zn]>[C:1]([C:4]1[CH:5]=[CH:6][C:7]2[CH2:8][C:9]3[C:14]([S:15](=[O:19])(=[O:18])[C:16]=2[CH:17]=1)=[CH:13][CH:12]=[CH:11][CH:10]=3)([OH:3])=[O:2]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 313Hydrochloric Acid3회HCID 401189-Oxo-9H-thioxanthene-3-carboxylic acid 10,10-dioxide

생성물 1

HCID 2038418310,10-Dioxo-9,10-dihydro-10lambda~6~-thioxanthene-3-carboxylic acid

시약·촉매·용매 2

HCID 23994Zinc촉매HCID 176Acetic Acid용매

실험 절차

3-Carboxythioxanthone-10,10-dioxide (prepared as in Reference Preparation 4) (5.0 g), zinc wool (10.0 g) and mercuric acetate (0.2 g) in acetic acid (100 ml) were brought to the boil and concentrated hydrochloric acid (10 ml) was added. Vigorous evolution of hydrogen chloride occurred at first. After 2 hr., further hydrochloric acid (7 ml), was added and the mixture boiled under reflux for further 4 hr. It was then filtered while hot and poured on to ice and water. The precipitated product was filtered off and dried at 80° C. in vacuo, m.p. 229°-248° C. Two recrystallisations from methanol gave the product m.p. 254° C.

후처리

  1. additionwas added
  2. temperatureunder reflux for further 4 hr
  3. filtrationIt was then filtered while hot and
  4. additionpoured on to ice and water
  5. filtrationThe precipitated product was filtered off
  6. customdried at 80° C. in vacuo, m.p. 229°-248° C
  7. customTwo recrystallisations from methanol

출처 및 근거

ORD 기록
ord-2daf1724912b4ab2b3d06b9a8ee65a21
출처 데이터셋
uspto-grants-1979_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04177257

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