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Phosphorus sulfide (P2S5) → 2H-Pyran-2-thione, 4,6-diphenyl-

HRID 1165285
ノート
印刷プレビュー

反応式

HRID 1165285 の反応式
[C:1]1([C:7]2[CH:12]=[C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[O:10][C:9](=O)[CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.P12(SP3(SP(SP(S3)(S1)=S)(=S)S2)=S)=[S:21]>C1C=CC=CC=1>[C:1]1([C:7]2[CH:12]=[C:11]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[O:10][C:9](=[S:21])[CH:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
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 2966854,6-diphenyl-2H-pyran-2-one

生成物 1

HCID 1861062H-Pyran-2-thione, 4,6-diphenyl-収率 134.2%

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

Under an inert atmosphere, 2.1 g of the product of Step A 45 ml of benzene and 7.5 g of phosphorus pentasulfide were mixed together and refluxed under inert atmosphere for 5 hours. Then the supernatant solution was decanted hot and concentrated to dryness by distilling under reduced pressure. This operation was repeated hot on the reaction medium four times, each time with 30 ml of benzene. The concentrates were put together and dried under a good vacuum to obtain 3 g of product which was chromatographed on silica and eluted with methylene chloride to obtain 2 g of the product sought melting at 122°-123° C.

後処理

  1. temperaturerefluxed under inert atmosphere for 5 hours
  2. customThen the supernatant solution was decanted hot
  3. concentrationconcentrated to dryness
  4. distillationby distilling under reduced pressure
  5. customdried under a good vacuum

出典と根拠

ORDレコード
ord-4de36a03eb69437e9c456d72aecbb8af
出典データセット
uspto-grants-1990_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04908359

反応ノート

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