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Cl.[CH3:2][CH2:3][CH:4]([N:7]([N:22]=[O:23])[C:8]1[C:13]([N+:14]([O-:16])=[O:15])=[C:12]([CH3:17])[C:11]([CH3:18])=[CH:10][C:9]=1[N+:19]([O-:21])=[O:20])[CH2:5][CH3:6]>>[CH3:2][CH2:3][CH:4]([NH:7][C:8]1[C:9]([N+:19]([O-:21])=[O:20])=[CH:10][C:11]([CH3:18])=[C:12]([CH3:17])[C:13]=1[N+:14]([O-:16])=[O:15])[CH2:5][CH3:6].[CH3:2][CH2:3][CH:4]([N:7]([N:22]=[O:23])[C:8]1[C:13]([N+:14]([O-:16])=[O:15])=[C:12]([CH3:17])[C:11]([CH3:18])=[CH:10][C:9]=1[N+:19]([O-:21])=[O:20])[CH2:5][CH3:6]참가 물질
실험 절차
A sample of crude Pendimethalin containing 18 weight percent of N-nitroso-pendimethalin was synthesized according to the procedure described in U.S. Pat. No. 4,621,157. Primary denitrosation was achieved by treating the crude, molten sample with a 5 molar excess of 37% HCl (based on contained N-nitroso-pendimethalin) at 105° C. After 1.5 hours, the concentration of N-nitroso-pendimethalin had decreased to <1.0 weight percent. The molten product was neutralized with dilute caustic and washed with hot water and cooled to room temperature. A 120 mg sample of the resulting solid was heated to 170° C. under 20 mm Hg vacuum for 15 minutes. The recovery of Pendimethalin was essentially quantitative and the concentration of N-nitroso-pendimethalin had decreased to 0.8 ppm.
후처리
- additionwith dilute caustic
- washwashed with hot water
- temperatureA 120 mg sample of the resulting solid was heated to 170° C. under 20 mm Hg vacuum for 15 minutes
출처 및 근거
- ORD 기록
- ord-0ca722a4586642f08f38fd094d362380
- 출처 데이터셋
- uspto-grants-1999_07
- 특허 번호
- US05922915
연결된 노트
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