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Water → 1-(2,4,6-Trichlorophenyl)-2-propanone O-methyloxime

HRID 2170299
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HRID 2170299 반응식
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[CH:5]=[C:4]([Cl:9])[C:3]=1[CH2:10][C:11](=O)[CH3:12].Cl.[CH3:15][O:16][NH2:17].O.[OH-].[Na+]>CO>[CH3:15][O:16][N:17]=[C:11]([CH3:12])[CH2:10][C:3]1[C:2]([Cl:1])=[CH:7][C:6]([Cl:8])=[CH:5][C:4]=1[Cl:9]
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6

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HCID 962WaterHCID 14798Sodium Hydroxide2회HCID 521874O-Methylhydroxylamine hydrochloride3회HCID 584436631-(2,4,6-Trichlorophenyl)-2-propanone

생성물 1

HCID 767875151-(2,4,6-Trichlorophenyl)-2-propanone O-methyloxime

시약·촉매·용매 1

HCID 887Methanol
용매

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온도
50 °C

실험 절차

1-(2,4,6-trichloro-phenyl)-propan-2-one (273 g, 1.118 mol) was suspended in methanol (544 g) at ambient temperature. The resulting suspension was then heated under stirring to a temperature of 50° C. (most of the solid is dissolved). Then O-methyl-hydroxylamine hydrochloride as a 30% solution in water (358 g, 1.286 mol) was fed within 30-60 min. maintaining the temperature between 50-52° C. During the course of O-methyl-hydroxylamine hydrochloride addition the reaction mass turned into a two-phase system (liquid-liquid). At the end of O-methyl-hydroxylamine hydrochloride feed the pH was adjusted to 4-5 by slow addition of NaOH 30% (264 g 1.981 mol). The mixture was then stirred for 1-2 hours at 50-52° C. to allow the reaction to go to completion. Subsequently the pH was adjusted to 7-8 by adding NaOH 30% (8.5 g, 0.064 mol).

후처리

  1. temperatureThe resulting suspension was then heated
  2. dissolutionis dissolved)
  3. temperaturemaintaining the temperature between 50-52° C
  4. stirringThe mixture was then stirred for 1-2 hours at 50-52° C.
  5. customthe reaction

출처 및 근거

ORD 기록
ord-e686b82ee35946d98986024f722dbc6a
출처 데이터셋
uspto-grants-2015_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09051272B2

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