Dimethylformamide → propargyl N-methoxy-2,4-dichlorobenzimidate

HRID 3405

反応式

HRID 3405 の反応式
[CH3:1][O:2][NH:3][C:4](=[O:13])[C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:6]=1[Cl:12].C(=O)([O-])[O-].[K+].[K+].[CH2:20](Br)[C:21]#[CH:22].CN(C)C=O>O>[CH3:1][O:2][N:3]=[C:4]([O:13][CH2:22][C:21]#[CH:20])[C:5]1[CH:10]=[CH:9][C:8]([Cl:11])=[CH:7][C:6]=1[Cl:12]

参加物

6

反応物 4

HCID 6228DimethylformamideHCID 7842Propargyl bromideHCID 11430Potassium CarbonateHCID 189350352,4-dichloro-N-methoxybenzamide

生成物 1

HCID 53654798propargyl N-methoxy-2,4-dichlorobenzimidate収率 29.8%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

1.0 g of N-methoxy-2,4-dichlorobenzamide, 0.75 g of potassium carbonate and 0.65 g of propargyl bromide were added to 10 ml of N,N-dimethylformamide, and the mixture was stirred for 3 hours. After completion of the reaction, water was added to the reaction solution, and the mixture was extracted with ethyl acetate. The extract was dried, concentrated and purified by silica gel column chromatography to obtain 0.35 g of propargyl N-methoxy-2,4-dichlorobenzimidate.

後処理

  1. additionwas added to the reaction solution
  2. extractionthe mixture was extracted with ethyl acetate
  3. customThe extract was dried
  4. concentrationconcentrated
  5. custompurified by silica gel column chromatography

出典と根拠

ORDレコード
ord-bc47ddbc82764811b755545cf676a4fc
出典データセット
uspto-grants-1998_03
特許番号
US05733935

関連ノート

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