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N,N-Dimethylglycine → N-(2-(2,5-Dimethyl-1-pyrrolyl)ethyl)-(N,N-dimethylamino)acetamide

HRID 1904229
ノート
印刷プレビュー

反応式

HRID 1904229 の反応式
[CH3:1][N:2]([CH2:4][C:5]([OH:7])=O)[CH3:3].C(N1C=CN=C1)(N1C=CN=C1)=O.[NH2:20][CH2:21][CH2:22][N:23]1[C:27]([CH3:28])=[CH:26][CH:25]=[C:24]1[CH3:29]>COCCOC>[CH3:29][C:24]1[N:23]([CH2:22][CH2:21][NH:20][C:5](=[O:7])[CH2:4][N:2]([CH3:3])[CH3:1])[C:27]([CH3:28])=[CH:26][CH:25]=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 673N,N-DimethylglycineHCID 682631,1'-CarbonyldiimidazoleHCID 137700502-(2,5-Dimethyl-1H-pyrrol-1-yl)ethan-1-amine

生成物 1

HCID 13770064N-(2-(2,5-Dimethyl-1-pyrrolyl)ethyl)-(N,N-dimethylamino)acetamide

試薬・触媒・溶媒 1

HCID 80711,2-Dimethoxyethane溶媒2 回

実験手順

5.2 g (0.05 mol) of N,N-dimethylaminoacetic acid and 8.1 g (0.05 mol) of carbonyldiimidazole in 20 ml of ethylene glycol dimethyl ether are stirred at 70° C. for 15 min. After addition of 5.5 g (0.04 mol) of 1-(2-aminoethyl)-2,5-dimethylpyrrole, dissolved in 20 ml of ethylene glycol dimethyl ether, to the mixture it is stirred at room temperature for 5 h, then concentrated, water is added, and the mixture is extracted first when acid and then when alkaline. The product contained in the extract from the mixture which has been made alkaline is crystallized using ligroin. Yield: 4.3 g (39% of theory), Melting point: 63°-65° C. Elemental analysis: C12H21N3O (223.32) calculated: C 64.5 H 9.5 N 18.8 O 7.2 found: C 64.0 H 9.4 N 18.5 O 8.0

後処理

  1. concentrationconcentrated
  2. additionwater is added
  3. extractionthe mixture is extracted first when acid
  4. extractionextract from the mixture which
  5. customis crystallized

出典と根拠

ORDレコード
ord-732bc9f7c96643e3aa7eb9ec59007b2f
出典データセット
uspto-grants-1989_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04837225

反応ノート

読み込み中…

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