Diisopropylethylamine → HCID 117830954、化合物

HRID 515928ノート

反応式

HRID 515928 の反応式
[CH3:1][N:2]1[CH:6]=[CH:5][C:4]([C:7]([OH:9])=O)=[C:3]1[CH3:10].ClC(N(C)C)=C(C)C.[CH2:19]([O:26][C:27]1[CH:34]=[CH:33][C:30]([NH:31][CH3:32])=[CH:29][CH:28]=1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1.C(N(C(C)C)C(C)C)C>ClCCCl.ClCCl>[CH2:19]([O:26][C:27]1[CH:28]=[CH:29][C:30]([N:31]([CH3:32])[C:7]([C:4]2[CH:5]=[CH:6][N:2]([CH3:1])[C:3]=2[CH3:10])=[O:9])=[CH:33][CH:34]=1)[C:20]1[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=1

参加物

7

反応物 4

HCID 81531DiisopropylethylamineHCID 6407921-Chloro-N,N-2-trimethylpropenylamineHCID 162176454-(Benzyloxy)-N-methylanilineHCID 225617641,2-dimethyl-1H-pyrrole-3-carboxylic acid

生成物 1

HCID 117830954HCID 117830954、化合物

試薬・触媒・溶媒 2

HCID 111,2-Dichloroethane溶媒2 回HCID 6344Dichloromethane溶媒

実験手順

To a suspension of 1,2-dimethylpyrrole-3-carboxylic acid (2.085 g; 15 mmol) in 1,2-dichloroethane (40 mL) there is added 1-chloro-N,N,2-trimethyl-prop-1-en-1-amine (2.37 mL; 17.9 mmol), and the solution formed is stirred for 1 hour. To the resulting solution there is added, dropwise, an ice-cold solution of 4-benzyloxy-N-methyl-aniline (3.73 g; 15 mmol) and N-ethyl-N-isopropyl-propan-2-amine (7.75 mL; 45 mmol) in 1,2-dichloroethane (40 mL). The reaction mixture is stirred at ambient temperature for 1 hour; it is then diluted with dichloromethane (250 mL) and washed with water (2×30 mL), dried over Na2SO4 and evaporated. The crude product is triturated with diethyl ether and the solid formed is filtered off to yield the title compound.

後処理

  1. customthe solution formed
  2. additionTo the resulting solution there is added
  3. stirringThe reaction mixture is stirred at ambient temperature for 1 hour
  4. washwashed with water (2×30 mL)
  5. dry with materialdried over Na2SO4
  6. customevaporated
  7. customThe crude product is triturated with diethyl ether
  8. customthe solid formed
  9. filtrationis filtered off

出典と根拠

ORDレコード
ord-33abba4a03ed46dabb45d2584086f89f
出典データセット
uspto-grants-2015_08
特許番号
US09108983B2

反応ノート

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