Sodium Carbonate → HCID 178488969, 화합물

HRID 235970노트

반응식

HRID 235970 반응식
[C:1]([C:4]1[N:5]=[C:6]([C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=2)[NH:7][CH:8]=1)(=O)[NH2:2].C([O-])([O-])=O.[Na+].[Na+]>O=P(Cl)(Cl)Cl>[C:1]([C:4]1[N:5]=[C:6]([C:9]2[CH:14]=[CH:13][C:12]([O:15][CH3:16])=[CH:11][CH:10]=2)[NH:7][CH:8]=1)#[N:2]

참가 물질

4

반응물 2

HCID 10340Sodium CarbonateHCID 178488972HCID 178488972, 화합물

생성물 1

HCID 178488969HCID 178488969, 화합물수율 71.7%

시약·촉매·용매 1

HCID 24813Phosphorus oxychloride용매

실험 절차

A mixture of 64 (7.6 g, 0.035 mol) and POCl3 (100 ml) was heated at reflux for 5.5 hours. After stirring at room temperature overnight, the suspension was poured into saturated Na2CO3 and the mixture extracted with 20% CH3OH--CHCl3 (3×). The organic extracts were washed with saturated NaCl, dried, filtered and concentrated to dryness. The residue was chromatographed on silica gel and the product eluted with 5% CH3OH--CHCl3 to yield 5.0 g (71%) of 65; m.p. 219°-20° C. (CH3CN).

후처리

  1. temperaturewas heated
  2. temperatureat reflux for 5.5 hours
  3. extractionthe mixture extracted with 20% CH3OH
  4. washThe organic extracts were washed with saturated NaCl
  5. customdried
  6. filtrationfiltered
  7. concentrationconcentrated to dryness
  8. customThe residue was chromatographed on silica gel
  9. washthe product eluted with 5% CH3OH

출처 및 근거

ORD 기록
ord-db0d841ebcff40da8b8d546fb8cf9489
출처 데이터셋
uspto-grants-1987_02
특허 번호
US04642311

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