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2-Methoxyethylamine → 2-Amino-5-(4-[2-methoxyethyl]aminophenylsulfonyloxy)nitrobenzene

HRID 1823762
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HRID 1823762 반응식
[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][S:9]([C:12]2[CH:17]=[CH:16][C:15](F)=[CH:14][CH:13]=2)(=[O:11])=[O:10])=[CH:4][C:3]=1[N+:19]([O-:21])=[O:20].[CH3:22][O:23][CH2:24][CH2:25][NH2:26]>O1CCOCC1>[NH2:1][C:2]1[CH:7]=[CH:6][C:5]([O:8][S:9]([C:12]2[CH:17]=[CH:16][C:15]([NH:26][CH2:25][CH2:24][O:23][CH3:22])=[CH:14][CH:13]=2)(=[O:11])=[O:10])=[CH:4][C:3]=1[N+:19]([O-:21])=[O:20]
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참가 물질

4

반응물 2

HCID 80182-MethoxyethylamineHCID 120188434-Amino-3-nitrophenyl 4-fluorobenzenesulfonate

생성물 1

HCID 120188472-Amino-5-(4-[2-methoxyethyl]aminophenylsulfonyloxy)nitrobenzene

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

반응 조건

온도
40 °C

실험 절차

15.6 g of 2-amino-5-(4-fluorophenylsulfonyloxy)nitrobenzene were combined with 35 ml methoxyethylamine in 100 ml dioxane in a round bottom flask. The reaction mixture was heated to reflux for 8 hours and then cooled to 40° C. and extracted two times with 250 ml water. Concentrate was solubilized with ethyl acetate and extracted with 2N aqueous HCl and water, the organic phase was then dried under reduced pressure, yielding 19.2 g of 2-amino-5-(4-[2-methoxyethyl]aminophenylsulfonyloxy)nitrobenzene (melting point 105° C.).

후처리

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 8 hours
  3. extractionextracted two times with 250 ml water
  4. concentrationConcentrate
  5. extractionextracted with 2N aqueous HCl and water
  6. customthe organic phase was then dried under reduced pressure

출처 및 근거

ORD 기록
ord-9c2c1c3f2c8a48109c5a6af8e6185440
출처 데이터셋
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07041668B2

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