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Water → 2,4-Dichloro-N-methoxy-N-methylbenzamide

HRID 605574
ノート
印刷プレビュー

反応式

HRID 605574 の反応式
Cl.[CH3:2][O:3][NH:4][CH3:5].C(N(CC)CC)C.[Cl:13][C:14]1[CH:22]=[C:21]([Cl:23])[CH:20]=[CH:19][C:15]=1[C:16](Cl)=[O:17].O>C(Cl)Cl>[Cl:13][C:14]1[CH:22]=[C:21]([Cl:23])[CH:20]=[CH:19][C:15]=1[C:16]([N:4]([O:3][CH3:2])[CH3:5])=[O:17]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 666452,4-Dichlorobenzoyl chlorideHCID 81138Methanamine, N-methoxy-, hydrochloride (1:1)

生成物 1

HCID 118453452,4-Dichloro-N-methoxy-N-methylbenzamide

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 32.6 g of N-methoxymethanamine hydrochloride and 91.2 ml of triethylamine in 500 ml of DCM is cooled in an ice bath, and then 47 ml of 2,4-dichlorobenzoyl chloride are added slowly and the mixture is left to stir while allowing the temperature to rise to AT. After stirring for 1 hour at AT, water is added to the reaction mixture, the mixture is extracted with DCM, the organic phase is dried over Na2SO4 and the solvent is evaporated under vacuum. 53 g of the expected compound are obtained.

後処理

  1. temperatureis cooled in an ice bath
  2. waitthe mixture is left
  3. additionis added to the reaction mixture
  4. extractionthe mixture is extracted with DCM
  5. dry with materialthe organic phase is dried over Na2SO4
  6. customthe solvent is evaporated under vacuum

出典と根拠

ORDレコード
ord-848fe4355e8c472db559bd1b7fe9dfa8
出典データセット
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07915258B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート