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Triethylamine → 1-(3-(4-Amino-2-(3,4,5-trimethoxyphenylamino)thieno[3,2-d]pyrimidin-7-yl)phenyl)-3-isopropylurea

HRID 1485494
ノート
印刷プレビュー

反応式

HRID 1485494 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([C:8]2[C:12]3[N:13]=[C:14]([NH:18][C:19]4[CH:24]=[C:23]([O:25][CH3:26])[C:22]([O:27][CH3:28])=[C:21]([O:29][CH3:30])[CH:20]=4)[N:15]=[C:16]([NH2:17])[C:11]=3[S:10][CH:9]=2)[CH:5]=[CH:6][CH:7]=1.C(N(CC)CC)C.[CH:38]([N:41]=[C:42]=[O:43])([CH3:40])[CH3:39].C(OCC)(=O)C>O1CCCC1>[NH2:17][C:16]1[C:11]2[S:10][CH:9]=[C:8]([C:4]3[CH:3]=[C:2]([NH:1][C:42]([NH:41][CH:38]([CH3:40])[CH3:39])=[O:43])[CH:7]=[CH:6][CH:5]=3)[C:12]=2[N:13]=[C:14]([NH:18][C:19]2[CH:24]=[C:23]([O:25][CH3:26])[C:22]([O:27][CH3:28])=[C:21]([O:29][CH3:30])[CH:20]=2)[N:15]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 8471TriethylamineHCID 8857Ethyl AcetateHCID 61277Isopropyl isocyanateHCID 532379637-(3-aminophenyl)-N2-(3,4,5-trimethoxyphenyl)thieno[3,2-d]pyrimidin-2,4-diamine

生成物 1

HCID 532381961-(3-(4-Amino-2-(3,4,5-trimethoxyphenylamino)thieno[3,2-d]pyrimidin-7-yl)phenyl)-3-isopropylurea収率 75.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

The 7-(3-aminophenyl)-N2-(3,4,5-trimethoxyphenyl)thieno[3,2-d]pyrimidin-2,4-diamine (20 mg, 0.047 mmol) synthesized in Example 11 was dissolved in anhydrous tetrahydrofuran (1 mL) and then triethylamine (20 μL, 0.14 mmol) and isopropyl isocyanate (5 mg, 0.057 mmol) were added. After stirring at room temperature for 4 hours, ethyl acetate (2 mL) was added and the mixture was washed with brine. After drying with MgSO4, the product was filtered and concentrated. Purification by silica gel chromatography (ethyl acetate/hexane, 1/1) yielded the target compound of Example 12 (18 mg, 75% yield).

後処理

  1. washthe mixture was washed with brine
  2. dry with materialAfter drying with MgSO4
  3. filtrationthe product was filtered
  4. concentrationconcentrated
  5. customPurification by silica gel chromatography (ethyl acetate/hexane, 1/1)

出典と根拠

ORDレコード
ord-27c370ef130847b7a310df68a21debcd
出典データセット
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09422307B2

反応ノート

読み込み中…

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