Hydrochloric Acid → 2-Acetylphenoxathiin

HRID 372485

反応式

HRID 372485 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][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]

参加物

7

反応物 4

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

生成物 1

HCID 5151742-Acetylphenoxathiin

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6348Carbon Disulfide溶媒

実験手順

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.

後処理

  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.

出典と根拠

ORDレコード
ord-fc1a691dec11435887507c279c0d51f7
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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