Hydrochloric Acid → 2-Acetylphenoxathiin

HRID 372485

반응식

HRID 372485 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][CH:2]=1.[C:15](Cl)(=[O:17])[CH3:16].[Cl-].[Al+3].[Cl-].[Cl-].Cl>C(=S)=S.O>[C:15]([C:10]1[CH:9]=[CH:8][C:7]2[O:6][C:5]3[C:14](=[CH:1][CH:2]=[CH:3][CH:4]=3)[S:13][C:12]=2[CH:11]=1)(=[O:17])[CH3:16]

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 6367Acetyl chlorideHCID 9217PhenoxathiinHCID 6451240Aluminum(III) Chloride

생성물 1

HCID 5151742-Acetylphenoxathiin

시약·촉매·용매 2

HCID 962Water용매HCID 6348Carbon Disulfide용매

실험 절차

Phenoxathiin (22.9 g) and acetyl chloride (8.8 ml) were dissolved in carbon disulphide (120 ml) and mechanically stirred while aluminium chloride (15.5 g) was added in small portions. The red mixture was stirred for 2 hr. at room temperature, then boiled under reflux on the water bath for a further 21/4 hours. The mixture was cooled and poured on to a mixture of ice and hydrochloric acid, and the precipitated product filtered off, washed with water, and recrystallised once from ethanol and twice from petroleum ether (b.p. 80°-100° C), m.p. 112° C.

후처리

  1. additionwas added in small portions
  2. customat room temperature
  3. temperatureThe mixture was cooled
  4. filtrationthe precipitated product filtered off
  5. washwashed with water
  6. customrecrystallised once from ethanol and twice from petroleum ether (b.p. 80°-100° C), m.p. 112° C.

출처 및 근거

ORD 기록
ord-fc1a691dec11435887507c279c0d51f7
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04091108

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