Sodium Chloride → HCID 20183383, 화합물

HRID 255724노트

반응식

HRID 255724 반응식
[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]

참가 물질

5

반응물 3

HCID 5234Sodium ChlorideHCID 24813Phosphorus oxychlorideHCID 11724425HCID 11724425, 화합물

생성물 1

HCID 20183383HCID 20183383, 화합물수율 66.6%

시약·촉매·용매 1

HCID 111,2-Dichloroethane용매

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-07b5bf4289ec46cc9f0d215685ed7a8f
출처 데이터셋
uspto-grants-1987_10
특허 번호
US04698340

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