Dabco → Chlorpyrifos

HRID 328186

反応式

HRID 328186 の反応式
[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]

参加物

9

反応物 5

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

生成物 1

HCID 2730Chlorpyrifos収率 97%

試薬・触媒・溶媒 3

HCID 66133Benzyl triethylammonium chloride触媒HCID 962Water溶媒HCID 6344Dichloromethane溶媒

反応条件

温度
42 °C

実験手順

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., .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).

後処理

  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

出典と根拠

ORDレコード
ord-3cd95343a7914640b2cc6a3c20f9eb5b
出典データセット
uspto-grants-1977_04
特許番号
US04016225

関連ノート

読み込み中…