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

HRID 2165615노트

반응식

HRID 2165615 반응식
[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

참가 물질

6

반응물 4

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b4635049c3d740aca719e174b0674c49
출처 데이터셋
uspto-grants-1990_07
특허 번호
US04940710

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