Potassium Carbonate → 4-(Ethylsulfanyl)-2,2,3,3-tetramethyl-2,3-dihydroazete

HRID 345751ノート

反応式

HRID 345751 の反応式
F[B-](F)(F)F.[CH2:6]([O+](CC)CC)[CH3:7].[CH3:13][C:14]1([CH3:21])[NH:17][C:16](=[S:18])[C:15]1([CH3:20])[CH3:19].C([O-])([O-])=O.[K+].[K+]>C(Cl)Cl>[CH2:6]([S:18][C:16]1[C:15]([CH3:20])([CH3:19])[C:14]([CH3:21])([CH3:13])[N:17]=1)[CH3:7]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 2723982Triethyloxonium tetrafluoroborateHCID 19911807HCID 19911807、化合物

生成物 1

HCID 144723344-(Ethylsulfanyl)-2,2,3,3-tetramethyl-2,3-dihydroazete

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒2 回

実験手順

To a solution of 10.5 ml of triethyloxonium tetrafluoroborate as a 1M solution in CH2Cl2, a solution of 1 g (7 mmol) of tetramethylazetidinethione in 3 ml of dry CH2Cl2 was added under an inert atmosphere. The mixture was stirred at room temperature for 1 hour and then at reflux for 1 hour. After cooling, it was added dropwise to 10 ml of a 50% K2CO3 solution at -10° C. After filtration, the organic phase was separated out and immediately dried over MgSO4. Filtration was followed by removal of the solvent under vacuum and the oily residue was subjected to flash silica chromatography (pet. ether: ethyl acetate; 8:2) to obtain the product as a colorless oil.

後処理

  1. temperatureat reflux for 1 hour
  2. temperatureAfter cooling
  3. filtrationAfter filtration
  4. customthe organic phase was separated out
  5. dry with materialimmediately dried over MgSO4
  6. filtrationFiltration
  7. customwas followed by removal of the solvent under vacuum

出典と根拠

ORDレコード
ord-0658cbe9d31c44f388e7b9966abe3413
出典データセット
uspto-grants-1991_10
特許番号
US05059596

反応ノート

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