Sodium Chloride → HCID 20183383、化合物

HRID 255724ノート

反応式

HRID 255724 の反応式
[CH3:1][C:2]1[N:7]=[C:6]([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[N:5]=[C:4]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:3]=1[C:23]([NH2:25])=O.[Cl-].[Na+].P(Cl)(Cl)(Cl)=O>ClCCCl>[CH3:1][C:2]1[N:7]=[C:6]([C:8]2[CH:9]=[CH:10][CH:11]=[CH:12][CH:13]=2)[N:5]=[C:4]([C:14]2[CH:19]=[CH:18][CH:17]=[C:16]([N+:20]([O-:22])=[O:21])[CH:15]=2)[C:3]=1[C:23]#[N:25]

参加物

5

反応物 3

HCID 5234Sodium ChlorideHCID 24813Phosphorus oxychlorideHCID 11724425HCID 11724425、化合物

生成物 1

HCID 20183383HCID 20183383、化合物収率 66.6%

試薬・触媒・溶媒 1

HCID 111,2-Dichloroethane溶媒

実験手順

A mixture of 6-methyl-4-(3-nitrophenyl)-2-phenyl-5-pyrimidinecarboxamide (10 g), sodium chloride (8 g) and phosphorous oxychloride (3.3 g) in 1,2-dichloroethane (50 ml) was refluxed for 10 hours. After removal of the sodium chloride, the reaction mixture was poured into a mixture of dichloromethane (200 ml) and aqueous saturated hydrogen carbonate solution (100 ml). The separated organic layer was dried over magnesium sulfate and evaporated in vacuo. The residue was crystallized from diethyl ether, collected, washed with diethyl ether and dried to give 6-methyl-4-(3-nitrophenyl)-2-phenyl-5-pyrimidinecarbonitrile (6.3 g).

後処理

  1. temperaturewas refluxed for 10 hours
  2. customAfter removal of the sodium chloride
  3. additionthe reaction mixture was poured into a mixture of dichloromethane (200 ml) and aqueous saturated hydrogen carbonate solution (100 ml)
  4. dry with materialThe separated organic layer was dried over magnesium sulfate
  5. customevaporated in vacuo
  6. customThe residue was crystallized from diethyl ether
  7. customcollected
  8. washwashed with diethyl ether
  9. customdried

出典と根拠

ORDレコード
ord-07b5bf4289ec46cc9f0d215685ed7a8f
出典データセット
uspto-grants-1987_10
特許番号
US04698340

反応ノート

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