Phosphorus sulfide (P2S5) → 2-(Thiophen-2-yl)ethanethioamide

HRID 52191

반응식

HRID 52191 반응식
[S:1]1[CH:5]=[CH:4][CH:3]=[C:2]1[CH2:6][C:7]([NH2:9])=O.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:11]>C1COCC1>[CH:4]1[CH:3]=[C:2]([CH2:6][C:7]([NH2:9])=[S:11])[S:1][CH:5]=1

참가 물질

4

반응물 2

HCID 14817Phosphorus sulfide (P2S5)HCID 78208Thiophen-2-acetamide

생성물 1

HCID 53119242-(Thiophen-2-yl)ethanethioamide수율 54.5%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution in THF (200 mL) of 2-thiopheneacetamide (4.04 g, 28.6 mmol), prepared as in step 1, was added P4S10 (12,7 g, 28.6 mmol), and the vigorously stirred reaction mixture was placed in a Bransonic 221 bath and irradiated with ultrasound for 30 min. The reaction mixture was filtered and the tiltrate was concentrated in vacuo. The crude product was taken up in CH2Cl2 and decanted from the solid residue. Pure 2-thiophenethioacetamide (2.45 g, 54% yield) was obtained by chromatography on silica gel (CH2Cl2).

후처리

  1. customthe vigorously stirred reaction mixture
  2. customirradiated with ultrasound for 30 min
  3. filtrationThe reaction mixture was filtered
  4. concentrationthe tiltrate was concentrated in vacuo
  5. customdecanted from the solid residue

출처 및 근거

ORD 기록
ord-1a3a301158814011a8b1f5c2bda94702
출처 데이터셋
uspto-grants-1997_04
특허 번호
US05616596

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