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Methyl 4-cyano-2-(4-ethylpiperazin-1-yl)-6-(m-tolylamino)pyrimidine-5-carboxylate → 2-(4-Ethylpiperazin-1-yl)-4-(m-tolylamino)-6,7-dihydro-5H-pyrrolo[3,4-d]pyrimidin-5-one

HRID 515968
ノート
印刷プレビュー

反応式

HRID 515968 の反応式
[C:1]([C:3]1[C:8]([C:9]([O:11]C)=O)=[C:7]([NH:13][C:14]2[CH:15]=[C:16]([CH3:20])[CH:17]=[CH:18][CH:19]=2)[N:6]=[C:5]([N:21]2[CH2:26][CH2:25][N:24]([CH2:27][CH3:28])[CH2:23][CH2:22]2)[N:4]=1)#[N:2]>[Pd].CCO.Cl>[CH2:27]([N:24]1[CH2:23][CH2:22][N:21]([C:5]2[N:6]=[C:7]([NH:13][C:14]3[CH:15]=[C:16]([CH3:20])[CH:17]=[CH:18][CH:19]=3)[C:8]3[C:9](=[O:11])[NH:2][CH2:1][C:3]=3[N:4]=2)[CH2:26][CH2:25]1)[CH3:28]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 1

HCID 58317563Methyl 4-cyano-2-(4-ethylpiperazin-1-yl)-6-(m-tolylamino)pyrimidine-5-carboxylate

生成物 1

HCID 532519482-(4-Ethylpiperazin-1-yl)-4-(m-tolylamino)-6,7-dihydro-5H-pyrrolo[3,4-d]pyrimidin-5-one収率 43%

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 313Hydrochloric Acid溶媒HCID 702Ethanol溶媒

実験手順

A mixture of methyl 4-cyano-2-(4-ethylpiperazin-1-yl)-6-(m-tolylamino)pyrimidine-5-carboxylate (49.8 mg, 0.131 mmol) and palladium on carbon (10.1 mg) in EtOH (3 mL) and 1N HCl (3 mL) was stirred at RT for 2 h under a hydrogen atmosphere. The insoluble materials were filtered off, and the filtrate was concentrated under reduced pressure. The residue was treated with saturated aq NaHCO3 and EtOAc for 3 h. The mixture was extracted with EtOAc. The organic layers were washed with aq NaHCO3, water, and brine, were dried over anhydrous Na2SO4, and then filtered. The filtrate was concentrated under reduced pressure and the residue was purified by column chromatography twice (SiO2, EtOAc then DM1020 EtOAc/MeOH=20/1) to give the title compound as a white solid (19.8 mg, 43%). 1H NMR (500 MHz, CDCl3) δ ppm 1.19 (br s, 3H), 2.36 (s, 3H), 2.5 (br s, 6H), 4.08 (br s, 4H), 4.23 (s, 2H), 5.50 (s, 1H), 6.91-6.92 (m, 1H), 7.22-7.26 (m, 1H), 7.49-7.54 (m, 2H), 8.44 (s, 1H). [M+H] calc'd for C19H25N6O, 353; found, 353.

後処理

  1. filtrationThe insoluble materials were filtered off
  2. concentrationthe filtrate was concentrated under reduced pressure
  3. additionThe residue was treated with saturated aq NaHCO3 and EtOAc for 3 h
  4. extractionThe mixture was extracted with EtOAc
  5. washThe organic layers were washed with aq NaHCO3, water, and brine
  6. dry with materialwere dried over anhydrous Na2SO4
  7. filtrationfiltered
  8. concentrationThe filtrate was concentrated under reduced pressure
  9. customthe residue was purified by column chromatography twice (SiO2, EtOAc

出典と根拠

ORDレコード
ord-3690a656a3704095a4256755d063d38a
出典データセット
uspto-grants-2015_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09108970B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート