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Pyridine → Ethyl 2-(2,4,5-trichlorophenyl)oxycarbonyloxyimino-2-cyanoacetate

HRID 1283760
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HRID 1283760 반응식
Cl[C:2]([O:4][N:5]=[C:6]([C:12]#[N:13])[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:3].[Cl:14][C:15]1[CH:20]=[C:19]([Cl:21])[C:18]([Cl:22])=[CH:17][C:16]=1[OH:23].N1C=CC=CC=1>C1C=CC=CC=1>[Cl:14][C:15]1[CH:20]=[C:19]([Cl:21])[C:18]([Cl:22])=[CH:17][C:16]=1[O:23][C:2]([O:4][N:5]=[C:6]([C:12]#[N:13])[C:7]([O:9][CH2:10][CH3:11])=[O:8])=[O:3]
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참가 물질

5

반응물 3

HCID 1049PyridineHCID 72712,4,5-TrichlorophenolHCID 53929971Ethyl 2-chlorocarbonyloxyimino-2-cyanoacetate

생성물 1

HCID 54542381Ethyl 2-(2,4,5-trichlorophenyl)oxycarbonyloxyimino-2-cyanoacetate수율 65.7%

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

To a solution of ethyl 2-chlorocarbonyloxyimino-2-cyanoacetate (0.05 mol) prepared as in Example 11 (1), a solution of 2,4,5-trichlorophenol (9.9 g) and pyridine (3.9 g) in benzene (50 ml) is dropwise added under cooling with icewater. The resulting mixture is stirred for 1 hour and allowed to stand over night. The reaction mixture is washed with water, dried and concentrated. The residue is admixed with petroleum ether and filtered to collect crystals, which is dried and recrystallized from a benzene-petroleum ether mixture to give ethyl 2-(2,4,5-trichlorophenyl)oxycarbonyloxyimino-2-cyanoacetate (12.0 g). M.P. 101 to 103°C.

후처리

  1. temperatureunder cooling with icewater
  2. waitto stand over night
  3. washThe reaction mixture is washed with water
  4. customdried
  5. concentrationconcentrated
  6. filtrationfiltered
  7. customto collect crystals, which
  8. customis dried
  9. customrecrystallized from a benzene-petroleum ether mixture

출처 및 근거

ORD 기록
ord-f7a2a26cccc8422891c3cb340c4cd9f2
출처 데이터셋
uspto-grants-1976_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US03976635

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