1-Methylpiperazine → 6-[(4-Methylpiperazin-1-yl)methyl]-5-(4-nitrophenyl)thieno[2,3-d]pyrimidin-4-amine

HRID 227607ノート

反応式

HRID 227607 の反応式
Br[CH2:2][C:3]1[S:12][C:6]2[N:7]=[CH:8][N:9]=[C:10]([NH2:11])[C:5]=2[C:4]=1[C:13]1[CH:18]=[CH:17][C:16]([N+:19]([O-:21])=[O:20])=[CH:15][CH:14]=1.[CH3:22][N:23]1[CH2:28][CH2:27][NH:26][CH2:25][CH2:24]1>CN(C=O)C>[CH3:22][N:23]1[CH2:28][CH2:27][N:26]([CH2:2][C:3]2[S:12][C:6]3[N:7]=[CH:8][N:9]=[C:10]([NH2:11])[C:5]=3[C:4]=2[C:13]2[CH:18]=[CH:17][C:16]([N+:19]([O-:21])=[O:20])=[CH:15][CH:14]=2)[CH2:25][CH2:24]1

参加物

4

反応物 2

HCID 531671-MethylpiperazineHCID 590995626-(Bromomethyl)-5-(4-nitrophenyl)thieno[2,3-d]pyrimidin-4-amine

生成物 1

HCID 116251676-[(4-Methylpiperazin-1-yl)methyl]-5-(4-nitrophenyl)thieno[2,3-d]pyrimidin-4-amine収率 33.1%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of Example 57A (330 mg) and N-methylpiperazine (0.3 mL, 2.71 mmol) in DMF (6 mL) was stirred at room temperature overnight and concentrated. The concentrate was absorbed on silica gel and purified by flash column chromatography with ethyl acetate followed by 12% methanol/dichloromethane to provide 115 mg the desired product. Rf=0.38 (12% methanol/dichloromethane).

後処理

  1. concentrationconcentrated
  2. customThe concentrate was absorbed on silica gel
  3. custompurified by flash column chromatography with ethyl acetate

出典と根拠

ORDレコード
ord-5abe58e1334e4a13a08db1de6bc4fb3b
出典データセット
uspto-grants-2009_07
特許番号
US07560552B2

反応ノート

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