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4-Nitrophenyl chloroformate → HCID 22890091, 화합물

HRID 966465
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HRID 966465 반응식
[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]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 821294-Nitrophenyl chloroformateHCID 92933beta-Hydroxyethyl sulfone

생성물 1

HCID 22890091HCID 22890091, 화합물

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-8a46816c05854fa0a825778316babb34
출처 데이터셋
uspto-grants-2005_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06951930B2

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