Sodium Carbonate → HCID 178488969、化合物

HRID 235970ノート

反応式

HRID 235970 の反応式
[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]

参加物

4

反応物 2

HCID 10340Sodium CarbonateHCID 178488972HCID 178488972、化合物

生成物 1

HCID 178488969HCID 178488969、化合物収率 71.7%

試薬・触媒・溶媒 1

HCID 24813Phosphorus oxychloride溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-db0d841ebcff40da8b8d546fb8cf9489
出典データセット
uspto-grants-1987_02
特許番号
US04642311

反応ノート

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