Dimethylformamide → HCID 20185099、化合物

HRID 2309360ノート

反応式

HRID 2309360 の反応式
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

参加物

7

反応物 4

HCID 6228DimethylformamideHCID 19660Carbonate IonHCID 27275201-Benzyl-3-methylpiperazineHCID 13557183HCID 13557183、化合物

生成物 1

HCID 20185099HCID 20185099、化合物収率 90.1%

試薬・触媒・溶媒 2

HCID 241Benzene溶媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-809c8fc7a5314bbdb583288528b07513
出典データセット
uspto-grants-1987_09
特許番号
US04695568

反応ノート

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