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

HRID 52191

反応式

HRID 52191 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 53119242-(Thiophen-2-yl)ethanethioamide収率 54.5%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-1a3a301158814011a8b1f5c2bda94702
出典データセット
uspto-grants-1997_04
特許番号
US05616596

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