Water → (+)-(4R)-4-acetylthiopyrrolidine-2-thione

HRID 2396876노트

반응식

HRID 2396876 반응식
C([C@H:4]1[CH2:8][NH:7][C:6](=[S:9])[CH2:5]1)(=O)C.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:11].O.[C:25]([O:28]CC)(=O)[CH3:26]>C1(C)C=CC=CC=1>[C:25]([S:11][C@H:4]1[CH2:8][NH:7][C:6](=[S:9])[CH2:5]1)(=[O:28])[CH3:26]

참가 물질

6

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 14817Phosphorus sulfide (P2S5)HCID 86748733(4R)-4-acetylthio-2-pyrrolidone

생성물 1

HCID 53742819(+)-(4R)-4-acetylthiopyrrolidine-2-thione수율 72%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

(4R)-4-Acetylthio-2-pyrrolidone (10 g) is dissolved in toluene (100 ml), and thereto is added gradually phosphorus pentasulfide (9.5 g), and the mixture is stirred at room temperature for 20 minutes. To the reaction solution are added water and ethyl acetate, and the mixture is stirred at room temperature for 1.5 hour. The insoluble materials are removed by filtration, and the organic layer is washed with water, dried, and evaporated to remove the solvent. The residue is recrystallized from toluene to give (+)-(4R)-4-acetylthiopyrrolidine-2-thione (7.9 g).

후처리

  1. stirringthe mixture is stirred at room temperature for 1.5 hour
  2. customThe insoluble materials are removed by filtration
  3. washthe organic layer is washed with water
  4. customdried
  5. customevaporated
  6. customto remove the solvent
  7. customThe residue is recrystallized from toluene

출처 및 근거

ORD 기록
ord-0efef8f5c3c74f5d89b7562938077ef7
출처 데이터셋
uspto-grants-1996_02
특허 번호
US05495012

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