Dimethylcarbamoyl Chloride → Urea, N,N-dimethyl-N-2-propynyl- (9CI)

HRID 600184ノート

反応式

HRID 600184 の反応式
[CH3:1][N:2]([CH3:6])[C:3](Cl)=[O:4].[CH2:7]([NH2:10])[C:8]#[CH:9].CN(C1C=CC=CN=1)C>N1C=CC=CC=1.C(OCC)(=O)C>[CH3:1][N:2]([CH3:6])[C:3]([NH:10][CH2:7][C:8]#[CH:9])=[O:4]

参加物

6

反応物 3

HCID 6598Dimethylcarbamoyl ChlorideHCID 218852-DimethylaminopyridineHCID 239041Propargylamine

生成物 1

HCID 44190381Urea, N,N-dimethyl-N-2-propynyl- (9CI)

試薬・触媒・溶媒 2

HCID 1049Pyridine溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Dimethyl carbamylchloride (0.84 mL, 9.1 μmmol) was added to a stirred solution of propargylamine (0.62 mL, 9.1 mmol) and dimethylaminopyridine (22 mg, 0.18 mmol) in pyridine (5 mL) at room temperature. The resulting suspension was stirred at ambient temperature for approximately 15 h. The reaction mixture was diluted with ethyl acetate and washed successively with 1N HCl and brine. The organic phase was dried (Na2SO4), filtered and concentrated in vacuo to afford the title compound (i-3), which was used without further purification.

後処理

  1. washwashed successively with 1N HCl and brine
  2. dry with materialThe organic phase was dried (Na2SO4)
  3. filtrationfiltered
  4. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-e73d60aa1093461792ddc3b483d53425
出典データセット
uspto-grants-2011_03
特許番号
US07901893B2

反応ノート

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