Water → 2-(3-Methylthiophen-2-YL)piperazine

HRID 2165615ノート

反応式

HRID 2165615 の反応式
[CH3:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[C:7](=O)[CH:8]=O.[CH2:11]([NH2:14])[CH2:12][NH2:13].[BH4-].[Na+].O>C(O)C>[CH3:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[CH:7]1[CH2:8][NH:14][CH2:11][CH2:12][NH:13]1

参加物

6

反応物 4

HCID 962WaterHCID 3301EthylenediamineHCID 4311764Sodium borohydrideHCID 230429823-Methyl-alpha-oxo-2-thiopheneacetaldehyde

生成物 1

HCID 197635922-(3-Methylthiophen-2-YL)piperazine

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

A 5 g portion of the above aldehyde was dissolved in 100 ml of ethanol, cooled to 0°-5° C. and a solution of 2.14 g of ethylenediamine in 10 ml of ethanol was added dropwise with stirring. The mixture was allowed to come to room temperature over 3 hours, then 2.4 g of sodium borohydride was added and the mixture was stirred for 18 hours. Water was added, then the mixture was concentrated. The residue was dissolved in dichloromethane, cooled, extracted with water, dried, filtered and evaporated to an oil which crystallized, giving 4.6 g of 2-(3-methyl-2-thienyl)piperazine.

後処理

  1. temperaturecooled to 0°-5° C.
  2. stirringthe mixture was stirred for 18 hours
  3. concentrationthe mixture was concentrated
  4. dissolutionThe residue was dissolved in dichloromethane
  5. temperaturecooled
  6. extractionextracted with water
  7. customdried
  8. filtrationfiltered
  9. customevaporated to an oil which
  10. customcrystallized

出典と根拠

ORDレコード
ord-b4635049c3d740aca719e174b0674c49
出典データセット
uspto-grants-1990_07
特許番号
US04940710

反応ノート

読み込み中…