Phosphorus sulfide (P2S5) → HCID 21256521、化合物

HRID 635794ノート

反応式

HRID 635794 の反応式
[CH2:1]([CH:3]1[C:8](=O)[NH:7][C:6]2[CH:10]=[CH:11][CH:12]=[CH:13][C:5]=2[O:4]1)[CH3:2].P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:15]>N1C=CC=CC=1>[CH2:1]([CH:3]1[C:8](=[S:15])[NH:7][C:6]2[CH:10]=[CH:11][CH:12]=[CH:13][C:5]=2[O:4]1)[CH3:2]

参加物

4

反応物 2

HCID 14817Phosphorus sulfide (P2S5)HCID 31555992-Ethyl-2H-benzo[b][1,4]oxazin-3(4H)-one

生成物 1

HCID 21256521HCID 21256521、化合物収率 532.7%

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

0.25 g of 2-ethyl-1,4-benzoxazin-3-one is stirred in 2 ml of pyridine with 95 mg of phosphorus pentasulfide. The reaction is completed by reflux-boiling. It is poured onto water, extracted with ethyl acetate, and the organic phase is washed with brine. It is dried with magnesium sulfate and concentrated by evaporation. After column chromatography with hexane/ethyl acetate, 220 mg of product results.

後処理

  1. temperatureby reflux-boiling
  2. additionIt is poured onto water
  3. extractionextracted with ethyl acetate
  4. washthe organic phase is washed with brine
  5. dry with materialIt is dried with magnesium sulfate
  6. concentrationconcentrated by evaporation

出典と根拠

ORDレコード
ord-97f59d314a304465accf2e88423a266d
出典データセット
uspto-grants-2001_02
特許番号
US06191127B1

反応ノート

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