Potassium Carbonate → HCID 14074112, 화합물

HRID 621507노트

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HRID 621507 반응식
Br.Br.[OH:3][C:4]1[C:9]([CH3:10])=[CH:8][C:7]([N:11]2[CH2:16][CH2:15][NH:14][CH2:13][CH2:12]2)=[CH:6][C:5]=1[CH3:17].Cl[C:19]1[C:24]([CH3:25])=[C:23]([CH3:26])[N:22]=[C:21]([C:27]2[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=2)[N:20]=1.C([O-])([O-])=O.[K+].[K+]>CN(C=O)C>[OH:3][C:4]1[C:5]([CH3:17])=[CH:6][C:7]([N:11]2[CH2:12][CH2:13][N:14]([C:19]3[C:24]([CH3:25])=[C:23]([CH3:26])[N:22]=[C:21]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=4)[N:20]=3)[CH2:15][CH2:16]2)=[CH:8][C:9]=1[CH3:10]

참가 물질

5

반응물 3

HCID 11430Potassium Carbonate3회HCID 134879354-Chloro-5,6-dimethyl-2-phenylpyrimidineHCID 21243172HCID 21243172, 화합물

생성물 1

HCID 14074112HCID 14074112, 화합물수율 76%

시약·촉매·용매 1

HCID 6228Dimethylformamide용매

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온도
90 °C

실험 절차

A mixture of 4.42 g (12 mmol) of 1-(4-hydroxy-3,5-dimethylphenyl)piperazine dihydrobromide, 2.84 g (13 mmole) of 4-chloro-5,6-dimethyl-2-phenylpyrimidine, 1.66 g (12 mmol) of powdered K2CO3 and 38 ml of absolute DMF was warmed to 90° C., and 277 mg of powdered K2CO3 were added at 90° C. with stirring in each case after 10 minutes, after a further 25 minutes and after a further 60 minutes (in total 6 mmol of K2CO3), and the mixture was stirred for a further 6 hours at 95° C. The DMF was subsequently removed by distillation in vacuo, the residue was taken up in CH2Cl2 /water, the phases were separated after through mixing, and the aqueous phase was extracted a further three times with CH2Cl2. The combined CH2Cl2 extracts were dried, filtered and evaporated in vacuo. The crystalline residue (5.2 g) was boiled with 15 ml of methanol, and the crystals were filtered off under suction after cooling in an ice bath. In this fashion, 3.54 g (=76% yield) of pure 1-(4-hydroxy-3,5-dimethylphenyl)-4-(5,6-dimethyl-2-phenylpyrimidin-4-yl)piperazine, melting point 188°-89° C., were obtained;

후처리

  1. customThe DMF was subsequently removed by distillation in vacuo
  2. customthe phases were separated after
  3. additionthrough mixing
  4. extractionthe aqueous phase was extracted a further three times with CH2Cl2
  5. dry with materialThe combined CH2Cl2 extracts were dried
  6. filtrationfiltered
  7. customevaporated in vacuo
  8. filtrationthe crystals were filtered off under suction
  9. temperatureafter cooling in an ice bath

출처 및 근거

ORD 기록
ord-2b69ccacd08f43c0bb9777b8c45a0948
출처 데이터셋
uspto-grants-1989_04
특허 번호
US04824846

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