Isoamyl Nitrite → HCID 178508438, 화합물

HRID 2081798

반응식

HRID 2081798 반응식
[Cl:1][C:2]1[N:7]=[C:6]([NH2:8])[N:5]=[C:4]([NH2:9])[C:3]=1[NH2:10].[N:11](OCCC(C)C)=O>O1CCOCC1>[Cl:1][C:2]1[C:3]2[NH:10][N:11]=[N:9][C:4]=2[N:5]=[C:6]([NH2:8])[N:7]=1

참가 물질

4

반응물 2

HCID 8053Isoamyl NitriteHCID 5005056-Chloropyrimidine-2,4,5-triamine

생성물 1

HCID 178508438HCID 178508438, 화합물수율 78.9%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A solution of 6-chloro-2,4,5-pyrimidinetriamine (10.94 g, 0.0686 mol) and isoamyl nitrite (9.20 ml, 0.0686 mol)in dioxane (500 ml, freshly purified by passage through basic alumina) was heated under nitrogen with stirring for 2 hours at 90°. The reaction mixture was cooled, treated with activated carbon, filtered, and concentrated to 150 ml. Petroleum ether (250 ml, bp 35-60°) was added. The precipitate was filtered, washed the petroleum ether (50 ml) and dried in vacuo over P2O5 at 40° for 16 hours to give 9.23 g of crude desired product which was then used in the next step.

후처리

  1. temperaturewas heated under nitrogen
  2. temperatureThe reaction mixture was cooled
  3. additiontreated with activated carbon
  4. filtrationfiltered
  5. concentrationconcentrated to 150 ml
  6. additionPetroleum ether (250 ml, bp 35-60°) was added
  7. filtrationThe precipitate was filtered
  8. washwashed the petroleum ether (50 ml)
  9. dry with materialdried in vacuo over P2O5 at 40° for 16 hours

출처 및 근거

ORD 기록
ord-d6b3d8a284e94b3bab37b5e6ba0c37aa
출처 데이터셋
uspto-grants-1993_02
특허 번호
US05185459

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