Dimethylformamide → HCID 20185099, 화합물

HRID 2309360노트

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HRID 2309360 반응식
Cl[C:2]1[N:3]=[C:4]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:5]2[CH:10]=[C:9]([CH3:11])[S:8][C:6]=2[N:7]=1.[CH2:18]([N:25]1[CH2:30][CH2:29][NH:28][CH:27]([CH3:31])[CH2:26]1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C(=O)([O-])[O-].CN(C)C=O>O.C1C=CC=CC=1>[CH2:18]([N:25]1[CH2:30][CH2:29][N:28]([C:2]2[N:3]=[C:4]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[C:5]3[CH:10]=[C:9]([CH3:11])[S:8][C:6]=3[N:7]=2)[CH:27]([CH3:31])[CH2:26]1)[C:19]1[CH:20]=[CH:21][CH:22]=[CH:23][CH:24]=1

참가 물질

7

반응물 4

HCID 6228DimethylformamideHCID 19660Carbonate IonHCID 27275201-Benzyl-3-methylpiperazineHCID 13557183HCID 13557183, 화합물

생성물 1

HCID 20185099HCID 20185099, 화합물수율 90.1%

시약·촉매·용매 2

HCID 241Benzene용매HCID 962Water용매

실험 절차

A mixture of 3 g of 2-chloro-6-methyl-4-phenyl-thieno[2,3-d]pyrimidine, 2.2 g of 1-benzyl-3-methylpiperazine, 1.1 g of sodum carbonate and 4 ml of dimethylformamide is reacted under reflux for 3 hours. After cooling, 80 ml of benzene and 80 ml of water are added and two layers are separated. The benzene layer is washed twice with 100 ml of water and then with saturated aqueous sodium chloride solution, and dried over anhydrous sodium sulfate. After distilling off benzene, purification of the product by silica gel chromatography using 180 g of silica gel and n-hexane/ethyl acetate (10:1) as an eluent is carried out. There is obtained 4.3 g of oily 2-(4-benzyl-2-methylpiperazinyl)-6-methyl-4-phenyl-thieno[2,3-d]pyrimidine.

후처리

  1. customis reacted
  2. temperatureunder reflux for 3 hours
  3. temperatureAfter cooling
  4. customtwo layers are separated
  5. washThe benzene layer is washed twice with 100 ml of water
  6. dry with materialwith saturated aqueous sodium chloride solution, and dried over anhydrous sodium sulfate
  7. distillationAfter distilling off
  8. custombenzene, purification of the product by silica gel chromatography

출처 및 근거

ORD 기록
ord-809c8fc7a5314bbdb583288528b07513
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04695568

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