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p-Toluenesulfonic acid → HCID 20367264、化合物

HRID 617056
ノート
印刷プレビュー

反応式

HRID 617056 の反応式
C([O:3][C:4](=O)[CH:5]=[C:6]([NH2:10])OCC)C.C1(C)C=CC(S(O)(=O)=O)=CC=1.[Cl:23][C:24]1[C:32]([Cl:33])=[CH:31][CH:30]=[CH:29][C:25]=1[CH2:26][NH:27][NH2:28]>C(O)C>[NH2:10][C:6]1[NH:28][N:27]([CH2:26][C:25]2[CH:29]=[CH:30][CH:31]=[C:32]([Cl:33])[C:24]=2[Cl:23])[C:4](=[O:3])[CH:5]=1
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 6101p-Toluenesulfonic acidHCID 278451beta-Aminobeta-ethoxyacrylic acid ethyl esterHCID 20367233[(2,3-Dichlorophenyl)methyl]hydrazine

生成物 1

HCID 20367264HCID 20367264、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

16.7 g of β-amino-β-ethoxyacrylic acid ethyl ester and 1 g of p-toluenesulphonic acid were dissolved in 100 ml of ethanol and 20.2 g of 2,3-dichlorobenzylhydrazine were added. After standing overnight at room temperature, the precipitate which had formed was filtered off and dissolved in 2 N sodium hydroxide solution. The alkaline solution was again extracted with ether and subsequently slightly acidified with dilute acetic acid. Hereupon the compound identified above precipitated and after recrystallisation from ethanol the melting point was 161°-162° C. Yield: 11 g (40%).

後処理

  1. customthe precipitate which had formed
  2. filtrationwas filtered off
  3. dissolutiondissolved in 2 N sodium hydroxide solution
  4. extractionThe alkaline solution was again extracted with ether
  5. customabove precipitated
  6. customafter recrystallisation from ethanol the melting point was 161°-162° C

出典と根拠

ORDレコード
ord-9f8ada6e0218469badff2663e4127bb3
出典データセット
uspto-grants-1978_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04076943

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