Dimethylamine → 3-bromo-7-dimethylsulfamoyl-10,11-dihydro-5H-dibenzo[a,d]-cyclohepten-5-one

HRID 2071734ノート

反応式

HRID 2071734 の反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:11][CH2:10][C:9]3[CH:12]=[CH:13][C:14]([S:16](F)(=[O:18])=[O:17])=[CH:15][C:8]=3[C:7](=[O:20])[C:6]=2[CH:21]=1.[CH3:22][NH:23][CH3:24]>O1CCOCC1>[Br:1][C:2]1[CH:3]=[CH:4][C:5]2[CH2:11][CH2:10][C:9]3[CH:12]=[CH:13][C:14]([S:16](=[O:18])(=[O:17])[N:23]([CH3:24])[CH3:22])=[CH:15][C:8]=3[C:7](=[O:20])[C:6]=2[CH:21]=1

参加物

4

反応物 2

HCID 674DimethylamineHCID 214121113-bromo-7-fluorosulfonyl-10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-one

生成物 1

HCID 214120943-bromo-7-dimethylsulfamoyl-10,11-dihydro-5H-dibenzo[a,d]-cyclohepten-5-one

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

3-Bromo-7-fluorosulfonyl-10,11-dihydro-5H-dibenzo[a,d]cyclohepten-5-one (2.5 g., 0.00677 mole) together with 30 ml. of 25% aqueous dimethylamine and 30 ml. of p-dioxane is heated to refluxing for 3 hours. The brown solution is evaporated to dryness under reduced pressure and the residue partitioned between benzene and water. After washing with water, the benzene layer is evaporated to dryness under reduced pressure, leaving 3-bromo-7-dimethylsulfamoyl-10,11-dihydro-5H-dibenzo[a,d]-cyclohepten-5-one as a tan solid, m.p. 142°-145° C., in a yield of 2.1 g. (80%). An analytical sample melts at 146°-148° C. after crystallizations from mixtures of benzene and hexane and from methanol.

後処理

  1. temperatureto refluxing for 3 hours
  2. customThe brown solution is evaporated to dryness under reduced pressure
  3. customthe residue partitioned between benzene and water
  4. washAfter washing with water
  5. customthe benzene layer is evaporated to dryness under reduced pressure

出典と根拠

ORDレコード
ord-7cce932f28284a46ad6d7b492a04473d
出典データセット
uspto-grants-1977_09
特許番号
US04048223

反応ノート

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