Dimethylformamide → 2-(3-Chloropropylsulfanyl)thiophene

HRID 1792499

反応式

HRID 1792499 の反応式
Br[CH2:2][CH2:3][CH2:4][Cl:5].[S:6]1[CH:10]=[CH:9][CH:8]=[C:7]1[SH:11].C(=O)([O-])[O-].[K+].[K+].CN(C)C=O>O.C(OCC)(=O)C>[Cl:5][CH2:4][CH2:3][CH2:2][S:11][C:7]1[S:6][CH:10]=[CH:9][CH:8]=1

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 80061-Bromo-3-chloropropaneHCID 11430Potassium CarbonateHCID 5226742-Thiophenethiol

生成物 1

HCID 220310762-(3-Chloropropylsulfanyl)thiophene

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8857Ethyl Acetate溶媒

実験手順

2.7 mL 1-bromo-3-chloropropane was added to a mixture of 2 mL thiophen-2-thiol, 5.86 g potassium carbonate and 40 mL N,N-dimethylformamide under ice-cooling and then stirred at room temperature for 2 hours. Ethyl acetate and water were added to the reaction solution, and the organic layer was separated, washed with water plus brine (×2) and then with brine and dried over anhydrous sodium sulfate. The drying agent was filtered off, and the filtrate was evaporated. The resulting residue was purified by silica gel column chromatography (hexane) to give 4.19 g of the title compound as a pale yellow oil.

後処理

  1. temperaturecooling
  2. customthe organic layer was separated
  3. washwashed with water plus brine (×2)
  4. dry with materialwith brine and dried over anhydrous sodium sulfate
  5. filtrationThe drying agent was filtered off
  6. customthe filtrate was evaporated
  7. customThe resulting residue was purified by silica gel column chromatography (hexane)

出典と根拠

ORDレコード
ord-e61ef03a6a7048389b3fabfde9a97bb5
出典データセット
uspto-grants-2006_07
特許番号
US07074801B1

関連ノート

読み込み中…