Toluene → N-Cyanoacetylethylcarbamate

HRID 68537

反応式

HRID 68537 の反応式
[C:1]([CH2:3][C:4]([OH:6])=O)#[N:2].[NH2:7][C:8]([O:10][CH2:11][CH3:12])=[O:9].C1(C)C=CC=CC=1.P(Cl)(Cl)(Cl)=O>O.CN(C=O)C>[C:1]([CH2:3][C:4]([NH:7][C:8]([O:10][CH2:11][CH3:12])=[O:9])=[O:6])#[N:2]

参加物

7

反応物 4

HCID 1140TolueneHCID 5641Carbamic acid, ethyl esterHCID 9740Cyanoacetic acidHCID 24813Phosphorus oxychloride

生成物 1

HCID 23112N-Cyanoacetylethylcarbamate収率 67%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

2-cyanoacetic acid (85 g, 1 mol) and ethyl aminoformate (89 g, 1 mol) were added to toluene (500 mL). To the mixture was slowly added phosphorus oxychloride (45 mL, 0.5 mol), and then added DMF (5 mL). The reaction was conducted at 70° C. for 2 h. After cooling, water (500 mL) was added to the reaction solution to quench phosphorus oxychloride. The reaction is filtered by suction. The filtered cake was washed with ethyl ether and dried to produce a white solid (104 g) in a yield of 67%.

後処理

  1. temperatureAfter cooling
  2. customto quench phosphorus oxychloride
  3. filtrationThe reaction is filtered by suction
  4. washThe filtered cake was washed with ethyl ether
  5. customdried

出典と根拠

ORDレコード
ord-710c1d615b944b7f9adc6d68cc7a8ce0
出典データセット
uspto-grants-2014_09
特許番号
US08822465B2

関連ノート

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