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4-Nitrophenyl chloroformate → HCID 22890091、化合物

HRID 966465
ノート
印刷プレビュー

反応式

HRID 966465 の反応式
[S:1]([CH2:7][CH2:8][OH:9])([CH2:4][CH2:5][OH:6])(=[O:3])=[O:2].Cl[C:11]([O:13][C:14]1[CH:19]=[CH:18][C:17]([N+:20]([O-:22])=[O:21])=[CH:16][CH:15]=1)=[O:12]>N1C=CC=CC=1>[OH:6][CH2:5][CH2:4][S:1]([CH2:7][CH2:8][O:9][C:11]([O:13][C:14]1[CH:15]=[CH:16][C:17]([N+:20]([O-:22])=[O:21])=[CH:18][CH:19]=1)=[O:12])(=[O:3])=[O: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 821294-Nitrophenyl chloroformateHCID 92933beta-Hydroxyethyl sulfone

生成物 1

HCID 22890091HCID 22890091、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒

実験手順

A solution of 2,2′-sulfonyldiethanol (4.85 g, 39.75 mmol) and p-nitrophenyl chloroformate (2.0 g, 9.92 mmol), in 20 ml of dry pyridine, was stirred for 2 h at room temperature and then evaporated to dryness. The residue was dissolved in 350 ml of ethyl acetate and washed with water (4×100 ml). The organic solution was dried over sodium sulfate, filtered and evaporated. The crude product was purified by silica gel chromatography, eluting with ethyl acetate. The pure product fractions were pooled and evaporated affording an oil: 0.68 g (22%) yield.

後処理

  1. customevaporated to dryness
  2. dissolutionThe residue was dissolved in 350 ml of ethyl acetate
  3. washwashed with water (4×100 ml)
  4. dry with materialThe organic solution was dried over sodium sulfate
  5. filtrationfiltered
  6. customevaporated
  7. customThe crude product was purified by silica gel chromatography
  8. washeluting with ethyl acetate
  9. customevaporated
  10. customaffording an oil
  11. custom0.68 g (22%) yield

出典と根拠

ORDレコード
ord-8a46816c05854fa0a825778316babb34
出典データセット
uspto-grants-2005_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06951930B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート