Thiophene → 3-oxo-2-(2-thienyl)-3,4-dihydro-2H-1,4-benzothiazine

HRID 5844

反応式

HRID 5844 の反応式
Cl[CH:2]1[C:7](=[O:8])[NH:6][C:5]2[CH:9]=[CH:10][CH:11]=[CH:12][C:4]=2[S:3]1.[S:13]1[CH:17]=[CH:16][CH:15]=[CH:14]1>C(Cl)Cl>[O:8]=[C:7]1[NH:6][C:5]2[CH:9]=[CH:10][CH:11]=[CH:12][C:4]=2[S:3][CH:2]1[C:14]1[S:13][CH:17]=[CH:16][CH:15]=1

参加物

4

反応物 2

HCID 8030ThiopheneHCID 122185992H-1,4-Benzothiazin-3(4H)-one, 2-chloro-

生成物 1

HCID 189844063-oxo-2-(2-thienyl)-3,4-dihydro-2H-1,4-benzothiazine収率 70.3%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-chloro-3-oxo-3,4-dihydro-2H-1,4-benzothiazine (9.38 g) and thiophene (7.91 g) in methylene chloride (250 ml) is added in portions stannic chloride (12. 2 g) at 0° to 5° C. After stirring at the same temperature for 45 minutes, the mixture is poured into ice water, and the organic layer is separated. The aqueous layer is extracted with ethyl acetate, and the ethyl acetate layer is combined with the above organic layer and distilled to remove the solvent. The resulting solid material is recrystallized from ethanol to give 3-oxo-2-(2-thienyl)-3,4-dihydro-2H-1,4-benzothiazine (8.17 g) as crystals.

後処理

  1. customthe organic layer is separated
  2. extractionThe aqueous layer is extracted with ethyl acetate
  3. distillationdistilled
  4. customto remove the solvent
  5. customThe resulting solid material is recrystallized from ethanol

出典と根拠

ORDレコード
ord-9f13dedfca454f268811c8281667b82c
出典データセット
uspto-grants-1993_09
特許番号
US05246929

関連ノート

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