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Hydrochloric Acid → 2-Propanone, 1-(2-nitrophenoxy)-

HRID 489469
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HRID 489469 반응식
[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[OH:10])([O-:3])=[O:2].Cl[CH2:12][C:13](=[O:15])[CH3:14].[Br-].[Na+].C(=O)(O)[O-].[Na+].Cl>[Cl-].C([N+](CCCC)(CCCC)C)CCC.O.C1(C)C=CC=CC=1>[N+:1]([C:4]1[CH:9]=[CH:8][CH:7]=[CH:6][C:5]=1[O:10][CH2:12][C:13](=[O:15])[CH3:14])([O-:3])=[O:2]
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참가 물질

9

반응물 5

HCID 313Hydrochloric AcidHCID 6571Chloroacetone2회HCID 69472-NitrophenolHCID 253881Sodium BromideHCID 516892Sodium Bicarbonate

생성물 1

HCID 792392-Propanone, 1-(2-nitrophenoxy)-

시약·촉매·용매 3

HCID 91822
Tributylmethylammonium chloride
촉매
HCID 962Water용매
HCID 1140Toluene용매

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온도
65 °C

실험 절차

The o-nitrophenoxyacetone is prepared by heating with agitation for five hours at about 65° C. a mixture which consists of 421.6 g (3.006 moles) of o-nitrophenol, 297.8 g (3.09 moles) of chloroacetone, 37.2 g (96%, 0.3615 moles) of sodium bromide, 277.2 g (3.3 moles) of sodium bicarbonate, 21.8 g (0.0647 moles) of aqueous tributylmethylammonium chloride (TBMAC), and 829 g of toluene. There is then added 9.0 g (0.093 mole) of additional chloroacetone to the mixture which is further heated at 65° C. for 2.5 hours (note, sample analysis indicated that the reaction was complete after 1.5 hours). There is then added, 570 g of water and the pH of the mixture is adjusted to 6.5–7 at 55° C. to 60° C. upon addition of 55 g of a 10% HCl solution. The phases are allowed to separate and the aqueous phase is removed.

후처리

  1. temperatureis further heated at 65° C. for 2.5 hours (note, sample analysis
  2. additionThere is then added
  3. customto separate
  4. customthe aqueous phase is removed

출처 및 근거

ORD 기록
ord-98cbcdae6c2545c8bc14097ac9f282d3
출처 데이터셋
uspto-grants-2005_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06977299B2

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