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Water → 2-chloro-4-(2'-methylpropionamido)-N,N-diethylbenzamide

HRID 1198205
ノート
印刷プレビュー

反応式

HRID 1198205 の反応式
[Cl:1][C:2]1[CH:10]=[C:9]([NH:11][C:12](=[O:16])[CH:13]([CH3:15])[CH3:14])[CH:8]=[CH:7][C:3]=1[C:4](Cl)=[O:5].[CH2:17]([NH:19][CH2:20][CH3:21])[CH3:18].O>C1COCC1>[Cl:1][C:2]1[CH:10]=[C:9]([NH:11][C:12](=[O:16])[CH:13]([CH3:15])[CH3:14])[CH:8]=[CH:7][C:3]=1[C:4]([N:19]([CH2:20][CH3:21])[CH2:17][CH3:18])=[O:5]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 962WaterHCID 8021DiethylamineHCID 216426352-Chloro-4-(2'-methylpropionamido)benzoyl chloride

生成物 1

HCID 191042772-chloro-4-(2'-methylpropionamido)-N,N-diethylbenzamide

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

The crude 2-chloro-4-(2'-methylpropionamido)benzoyl chloride from the preceding reaction in dry THF (10 ml) was added dropwise with stirring over 10-15 minutes to a solution of diethylamine (1.46 g) in dry THF (10 ml), at 0°-5° C. After stirring at 0°-10° C. the reaction mixture was stood overnight at room temperature, poured into cold water and extracted with ethyl acetate. This extract was dried and evaporated to give a viscous gum which crystallised slowly and was then recrystallised from ethyl acetate to give 2-chloro-4-(2'-methylpropionamido)-N,N-diethylbenzamide as white crystals (0.507 g).

後処理

  1. additionwas added dropwise
  2. extractionextracted with ethyl acetate
  3. customThis extract was dried
  4. customevaporated
  5. customto give a viscous gum which
  6. customcrystallised slowly
  7. customwas then recrystallised from ethyl acetate

出典と根拠

ORDレコード
ord-0c20b4d4ea044229b1fac8acf9be02c2
出典データセット
uspto-grants-1994_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05280044

反応ノート

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