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HCID 18925402, 화합물 → HCID 18925404, 화합물

HRID 1289076
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HRID 1289076 반응식
[N+:1]([C:4]1[CH:8]=[CH:7][S:6][C:5]=1[C:9]1[CH:14]=[CH:13][C:12]([Cl:15])=[CH:11][CH:10]=1)([O-])=O>[Fe].C(O)(=O)C>[NH2:1][C:4]1[CH:8]=[CH:7][S:6][C:5]=1[C:9]1[CH:10]=[CH:11][C:12]([Cl:15])=[CH:13][CH:14]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 18925402HCID 18925402, 화합물

생성물 1

HCID 18925404HCID 18925404, 화합물수율 62%

시약·촉매·용매 2

HCID 23925Iron촉매HCID 176Acetic Acid용매

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온도
60 °C

실험 절차

To 20 ml of acetic acid, 1 g of 3-nitro-2-(4-chlorophenyl)thiophene and 0.93 g of iron powder were added and heated for 2 hours at 60° C. The reaction mixture was filtered through a diatomaceous earth (Celite) layer. Ethyl acetate was added to the filtrate and extracted 5 times with a 5% aqueous hydrogen chloride solution. The aqueous layer was neutralized with sodium hydrogen carbonate and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressure to obtain 0.54 g of the product as an yellow brown crystal. The yield was 62%. 1H-NMR(CDCl3, δ value):3.82(2H, brs), 6.64(1H, d, J=5.1), 7.12(1H, d, J=5.1), 7.34-7.39(2H, m), 7.43-7.48(2H, m)

후처리

  1. filtrationThe reaction mixture was filtered through a diatomaceous earth (Celite) layer
  2. additionEthyl acetate was added to the filtrate
  3. extractionextracted 5 times with a 5% aqueous hydrogen chloride solution
  4. extractionextracted with ethyl acetate
  5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
  6. distillationThe solvent was distilled off under reduced pressure

출처 및 근거

ORD 기록
ord-2a92a78c2bba40a8944d5cacdaaf4156
출처 데이터셋
uspto-grants-1998_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05747518

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