Potassium Carbonate → methoxycarbonylmethyl P-ethyl-2-nitro-5-(3,5-dichloro-2-pyridyloxy)phenylphosphinate

HRID 1284436

반응식

HRID 1284436 반응식
[CH2:1]([P:3]([C:6]1[CH:11]=[C:10]([O:12][C:13]2[C:18]([Cl:19])=[CH:17][C:16]([Cl:20])=[CH:15][N:14]=2)[CH:9]=[CH:8][C:7]=1[N+:21]([O-:23])=[O:22])(=[O:5])[OH:4])[CH3:2].C(=O)([O-])[O-].[K+].[K+].Br[CH2:31][C:32]([O:34][CH3:35])=[O:33]>CC(=O)CC>[CH2:1]([P:3]([C:6]1[CH:11]=[C:10]([O:12][C:13]2[C:18]([Cl:19])=[CH:17][C:16]([Cl:20])=[CH:15][N:14]=2)[CH:9]=[CH:8][C:7]=1[N+:21]([O-:23])=[O:22])(=[O:4])[O:5][CH2:31][C:32]([O:34][CH3:35])=[O:33])[CH3:2]

참가 물질

5

반응물 3

HCID 11430Potassium CarbonateHCID 60984Methyl bromoacetateHCID 20251602P-ethyl-2-nitro-5-(3,5-dichloro-2-pyridyloxy)phenylphosphinic acid

생성물 1

HCID 54154437methoxycarbonylmethyl P-ethyl-2-nitro-5-(3,5-dichloro-2-pyridyloxy)phenylphosphinate

시약·촉매·용매 1

HCID 6569Methyl Ethyl Ketone용매

실험 절차

A mixture of P-ethyl-2-nitro-5-(3,5-dichloro-2-pyridyloxy)phenylphosphinic acid (0.42 g., 1.2 mmol), potassium carbonate (2.0 mg), methyl bromoacetate (0.2 ml., 2.4 mmol), and 2-butanone (20 ml.) is heated under reflux for 2 hours. The reaction mixture is filtered and concentrated, and the crude product is purified by prep. TLC (50% ethyl acetate/hexane) to give methoxycarbonylmethyl P-ethyl-2-nitro-5-(3,5-dichloro-2-pyridyloxy)phenylphosphinate.

후처리

  1. temperatureis heated
  2. temperatureunder reflux for 2 hours
  3. filtrationThe reaction mixture is filtered
  4. concentrationconcentrated
  5. customthe crude product is purified by prep

출처 및 근거

ORD 기록
ord-9606fa63333e45f8a4164ce1fdc848a7
출처 데이터셋
uspto-grants-1986_01
특허 번호
US04563310

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