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Phosphorus sulfide (P2S5) → 4-Thioacetamidophenethyl Acetate

HRID 369565
ノート
印刷プレビュー

反応式

HRID 369565 の反応式
[C:1]([O:4][CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([NH:13][C:14](=O)[CH3:15])=[CH:9][CH:8]=1)(=[O:3])[CH3:2].P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:18]>C1(C)C=CC=CC=1>[C:1]([O:4][CH2:5][CH2:6][C:7]1[CH:12]=[CH:11][C:10]([NH:13][C:14](=[S:18])[CH3:15])=[CH:9][CH:8]=1)(=[O:3])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14817Phosphorus sulfide (P2S5)HCID 125713974-Acetamidophenethyl acetate

生成物 1

HCID 232822924-Thioacetamidophenethyl Acetate収率 142.3%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

4-Acetamidophenethyl acetate (10.0 g, 45.2 mmol) and phosphorus pentasulfide (10.0 g, 22.5 mmol) were suspended in toluene (200 ml). The suspension was refluxed for 40 min. After cooling the supernatant was decanted into a separatory funnel and washed with 50% aqueous Na2CO3 solution (70 ml) and then with water (70 ml). The organic toluene layer was dried over anhydrous sodium sulfate overnight. The dried toluene solution was concentrated to dryness to give a yellowish solid (7.6 g, 71%). This solid was used for next reaction without further purification.

後処理

  1. temperatureThe suspension was refluxed for 40 min
  2. temperatureAfter cooling the supernatant
  3. customwas decanted into a separatory funnel
  4. washwashed with 50% aqueous Na2CO3 solution (70 ml)
  5. dry with materialThe organic toluene layer was dried over anhydrous sodium sulfate overnight
  6. concentrationThe dried toluene solution was concentrated to dryness

出典と根拠

ORDレコード
ord-f4daf685128d4de4bd28c30416207fa9
出典データセット
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06140051

反応ノート

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