Potassium Hydroxide → Clomazone

HRID 1608482

반응식

HRID 1608482 반응식
Cl[CH2:2][C:3]([CH3:17])([CH3:16])[C:4]([N:6]([CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][C:10]=1[Cl:15])[OH:7])=[O:5].[OH-].[K+]>CO>[Cl:15][C:10]1[CH:11]=[CH:12][CH:13]=[CH:14][C:9]=1[CH2:8][N:6]1[C:4](=[O:5])[C:3]([CH3:17])([CH3:16])[CH2:2][O:7]1

참가 물질

4

반응물 2

HCID 14797Potassium HydroxideHCID 99255583-chloro-N-(2-chlorophenyl)methyl-N-hydroxy-2,2-dimethylpropanamide

생성물 1

HCID 54778Clomazone수율 0.1%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

One method for production of COMMAND® is disclosed in U.S. Pat. No. 4,405,357. Such preparation includes adding to a stirred solution of 6.3 grams (0,023 mole) of 3-chloro-N-(2-chlorophenyl)methyl-N-hydroxy-2,2-dimethylpropanamide in 45 ml of methanol dropwise a solution of 1.5 grams (0.023 mole) KOH (85% pure) in 25 ml methanol. The addition required 15 minutes and the temperature rose from 24° to 32° C. Upon completion of addition the reaction mixture was stirred for 18 hours at ambient temperature. By-product KCl was removed by filtering the mixture. The filtrate was poured into 500 ml of ice-water. The mixture was extracted with two portions of 250 ml each of methylene chloride. The combined extracts were dried with MgSO4 and filtered. Under reduced pressure the filtrate was concentrated to give 5.2 grams of 2-(2-chlorophenyl)methyl-4,4-dimethyl-3-isoxazolidinone as an oil.

후처리

  1. customSuch preparation
  2. additionThe addition required 15 minutes
  3. customrose from 24° to 32° C
  4. additionUpon completion of addition the reaction mixture
  5. customBy-product KCl was removed
  6. filtrationby filtering the mixture
  7. additionThe filtrate was poured into 500 ml of ice-water
  8. extractionThe mixture was extracted with two portions of 250 ml each of methylene chloride
  9. dry with materialThe combined extracts were dried with MgSO4
  10. filtrationfiltered
  11. concentrationUnder reduced pressure the filtrate was concentrated

출처 및 근거

ORD 기록
ord-9253409796da4ed691ce75ab75a92809
출처 데이터셋
uspto-grants-1995_03
특허 번호
US05395816

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