Potassium Hydroxide → Clomazone

HRID 1608482

反応式

HRID 1608482 の反応式
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

参加物

4

反応物 2

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

生成物 1

HCID 54778Clomazone収率 0.1%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-9253409796da4ed691ce75ab75a92809
出典データセット
uspto-grants-1995_03
特許番号
US05395816

関連ノート

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