Toluene → N-Cyanoacetylethylcarbamate

HRID 68537

반응식

HRID 68537 반응식
[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]

참가 물질

7

반응물 4

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

생성물 1

HCID 23112N-Cyanoacetylethylcarbamate수율 67%

시약·촉매·용매 2

HCID 962Water용매HCID 6228Dimethylformamide용매

실험 절차

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%.

후처리

  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

출처 및 근거

ORD 기록
ord-710c1d615b944b7f9adc6d68cc7a8ce0
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822465B2

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