Dabco → Chlorpyrifos

HRID 372668

반응식

HRID 372668 반응식
[P:1](=[S:9])(Cl)([O:5][CH2:6][CH3:7])[O:2][CH2:3][CH3:4].[Cl:10][C:11]1[C:12](C([O-])=O)=[N:13][C:14]([Cl:18])=[C:15]([Cl:17])[CH:16]=1.[Na+].C1N2CCN(CC2)C1.[OH-].[Na+].B([O-])([O-])[O-:34].[Na+].[Na+].[Na+]>[Cl-].C([N+](CC)(CC)CC)C1C=CC=CC=1.O.C(Cl)Cl>[CH3:4][CH2:3][O:2][P:1]([O:34][C:12]1[C:11]([Cl:10])=[CH:16][C:15]([Cl:17])=[C:14]([Cl:18])[N:13]=1)([O:5][CH2:6][CH3:7])=[S:9]

참가 물질

9

반응물 5

HCID 9237DabcoHCID 14798Sodium HydroxideHCID 17305O,O-diethyl phosphorochloridothioateHCID 159383boric acid, sodium saltHCID 23699972Sodium 3,5,6-trichloropyridinate

생성물 1

HCID 2730Chlorpyrifos수율 97%

시약·촉매·용매 3

HCID 66133Benzyl triethylammonium chloride촉매HCID 962Water용매HCID 6344Dichloromethane용매

반응 조건

온도
42 °C

실험 절차

O,O-Diethyl phosphorochloridothioate (11.3 g., 0.06 mole) was added dropwise to a stirred mixture of (1) sodium 3,5,6-trichloro-2-pyridinate (13.2 g., 0.06 mole) in 30 ml. of methylene chloride and 74 ml. of water, (2) 1 mole percent triethylene diamine, (3) 1 mole percent benzyltriethylammonium chloride and (4) a pH buffer consisting of NaOH and sodium borate. The stirred reaction mixture was maintained at 42° C. for 1.5 hours, cooled to room temperature, and the organic phase separated from the aqueous phase. The organic phase was washed once with approximately 30 ml. water and the organic solvent removed under reduced pressure. The title compound was thus obtained in 97 percent yield, based on 100 percent conversion of starting materials. The product was of excellent purity (approximately 99% pure).

후처리

  1. customThe stirred reaction mixture
  2. temperaturecooled to room temperature
  3. customthe organic phase separated from the aqueous phase
  4. washThe organic phase was washed once with approximately 30 ml
  5. customwater and the organic solvent removed under reduced pressure

출처 및 근거

ORD 기록
ord-e2c5fe5102bb47d589f53de7466bdb0a
출처 데이터셋
uspto-grants-1978_05
특허 번호
US04092312

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