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N,N-Dimethylaniline → 2-(beta,beta,beta-Trichloroethoxycarbonyl)amino-4-formylthiazole

HRID 979671
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반응식

HRID 979671 반응식
[Cl:1][C:2]([Cl:12])([Cl:11])[CH2:3][O:4][C:5]([NH:7][C:8]([NH2:10])=[S:9])=[O:6].BrC(Br)C(CBr)=[O:16].CN(C)[C:22]1[CH:27]=CC=C[CH:23]=1>C(O)C>[Cl:12][C:2]([Cl:1])([Cl:11])[CH2:3][O:4][C:5]([NH:7][C:8]1[S:9][CH:23]=[C:22]([CH:27]=[O:16])[N:10]=1)=[O:6]
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참가 물질

5

반응물 3

HCID 949N,N-DimethylanilineHCID 3146661,1,3-Tribromo-2-propanoneHCID 130920372,2,2-Trichloroethyl carbamothioylcarbamate

생성물 1

HCID 127632072-(beta,beta,beta-Trichloroethoxycarbonyl)amino-4-formylthiazole

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A solution of 10.0 g of N-(β,β,β-trichloroethoxycarbonyl)thiourea, 12.0 g. of 1,1,3-tribromoacetone and 5.0 g. of dimethylaniline in 100 ml. of ethanol is heated under reflux for 2 hours. After cooling, ethanol is removed under reduced pressure, and the oily residue is dissolved in ethyl acetate. Ethyl acetate layer is washed with water and dried over MgSO4. Ethyl acetate is removed under reduced pressure and the oily residue is dissolved in small quantity of chloroform. From the solution which is allowed to stand at room temperature is obtained 2-(β,β,β-trichloroethoxycarbonyl)amino-4-formylthiazole as a crystalline form. 5.0 g.

후처리

  1. temperatureunder reflux for 2 hours
  2. temperatureAfter cooling
  3. customethanol is removed under reduced pressure
  4. dissolutionthe oily residue is dissolved in ethyl acetate
  5. washEthyl acetate layer is washed with water
  6. dry with materialdried over MgSO4
  7. customEthyl acetate is removed under reduced pressure
  8. dissolutionthe oily residue is dissolved in small quantity of chloroform
  9. customto stand at room temperature

출처 및 근거

ORD 기록
ord-532c2feb0b444d31bb090d63d0a09df4
출처 데이터셋
uspto-grants-1987_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04668783

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