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

HRID 1534005ノート

反応式

HRID 1534005 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 reflux for 1 hour. After cooling, it was added dropwise to 10 mol 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. temperaturereflux 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-55d18a17d9fa4f6d8b8421dd36768904
出典データセット
uspto-grants-1992_02
特許番号
US05086170

反応ノート

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