Hydrazine → HCID 11241897, 화합물

HRID 230724노트

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HRID 230724 반응식
BrC1C=CC(Br)=CN=1.NN.[Br:11][C:12]1[CH:13]=[CH:14][C:15]([NH:18]N)=[N:16][CH:17]=1.N(C1C=CC=CN=1)N.[CH3:28][CH:29]([CH3:33])[C:30](=O)[CH3:31]>COCCO.C1C=CC=CC=1>[Br:11][C:12]1[CH:13]=[C:14]2[C:29]([CH3:33])([CH3:28])[C:30]([CH3:31])=[N:18][C:15]2=[N:16][CH:17]=1

참가 물질

8

반응물 5

HCID 9321HydrazineHCID 112513-Methyl-2-butanoneHCID 693532,5-DibromopyridineHCID 786452-HydrazinopyridineHCID 115356995-Bromo-2-hydrazinopyridine

생성물 1

HCID 11241897HCID 11241897, 화합물

시약·촉매·용매 2

HCID 241Benzene용매HCID 80192-Methoxyethanol용매

반응 조건

온도
110 °C

실험 절차

To 40 g of 2,5-dibromopyridine in 200 mL of 2-methoxyethanol is added 53 mL of anhydrous hydrazine and the mixture is heated at 110° C. for 3 hours to generate the 5-bromo-2-hydrazinopyridine. A mixture of 10 g of this hydrazinopyridine is heated at reflux overnight with 11 mL of 3-methyl-2-butanone in 40 mL of benzene equipped, using a condenser equipped with a Dean-Stark trap. All of the volatile components are removed under reduced pressure and the resulting residue is heated in 62 g of polyphosphoric acid at 140° C. for 45 minutes. The reaction mixture is poured into water, neutralized with sodium hydroxide and extracted with ethyl acetate. The resulting crude residue is purified by chromatography on silica gel, eluting with 1:1 ethyl acetate/hexanes, to yield 1.44 g of the product.

후처리

  1. temperatureis heated
  2. customequipped
  3. customequipped with a Dean-Stark trap
  4. customAll of the volatile components are removed under reduced pressure
  5. temperaturethe resulting residue is heated in 62 g of polyphosphoric acid at 140° C. for 45 minutes
  6. additionThe reaction mixture is poured into water
  7. extractionextracted with ethyl acetate
  8. customThe resulting crude residue is purified by chromatography on silica gel
  9. washeluting with 1:1 ethyl acetate/hexanes

출처 및 근거

ORD 기록
ord-585e5c5d338543c5bcd0462bd84d2af0
출처 데이터셋
uspto-grants-2009_07
특허 번호
US07566790B2

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