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Acetic Acid → 2-(4-Chloro-2-methoxypyridin-3-yl)-6-isopropylimidazo[4,5-f]isoindole-5,7(1H,6H)-dione

HRID 920494
ノート
印刷プレビュー

反応式

HRID 920494 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][C:10]=1[N+:11]([O-])=O)[C:7](=[O:14])[N:6]([CH:15]([CH3:17])[CH3:16])[C:5]2=[O:18].CC(O)=O.[Cl:23][C:24]1[C:29]([CH:30]=O)=[C:28]([O:32][CH3:33])[N:27]=[CH:26][CH:25]=1>CO>[Cl:23][C:24]1[CH:25]=[CH:26][N:27]=[C:28]([O:32][CH3:33])[C:29]=1[C:30]1[NH:11][C:10]2=[CH:9][C:8]3[C:7](=[O:14])[N:6]([CH:15]([CH3:17])[CH3:16])[C:5](=[O:18])[C:4]=3[CH:3]=[C:2]2[N:1]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 176Acetic AcidHCID 534079284-Chloro-2-methoxypyridine-3-carbaldehydeHCID 666902745-Amino-2-isopropyl-6-nitroisoindoline-1,3-dione

生成物 1

HCID 666894972-(4-Chloro-2-methoxypyridin-3-yl)-6-isopropylimidazo[4,5-f]isoindole-5,7(1H,6H)-dione収率 41.8%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

反応条件

温度
-50 °C

実験手順

To a suspension of 5-amino-2-isopropyl-6-nitroisoindoline-1,3-dione (0.37 g) in 250 mL of MeOH was added 5 mL of AcOH. The resulting solution was degassed with argon and then charged with 10% Pd/C (0.12 g, 50% wet) and hydrogenated at 40 psi of hydrogen for 16 h. Another 2 mL of AcOH was added to the mixture and then solids were filtered off. The filtrate was cooled to −50° C. and a solution of 4-chloro-2-methoxynicotinaldehyde (0.31 g, 1.78 mmol) in 200 mL of MeOH was added dropwise under inert atmosphere. The resulting solution was allowed to warm up to rt and stirred for 16 h. Solvent was evaporated and the oily residue was purified by column chromatography (7.5% MeOH in dichloromethane) to give title compound as a solid (0.23 g, 29.3%). 1H NMR (500 MHz, CDCl3) δ58.18 (s, 1H), 8.12 (d, 1H), 8.03 (s, 1H), 7.90 (d, 1H), 6.92 (d, 1H), 6.75 (d, 1H), 5.39 (s, 2H), 4.56 (p, 1H), 3.72 (s, 3H), 3.61 (s, 3H), 1.50 (d, 6H). ESI MS: m/z 371.1 (M+1).

後処理

  1. customThe resulting solution was degassed with argon
  2. additioncharged with 10% Pd/C (0.12 g, 50% wet) and hydrogenated at 40 psi of hydrogen for 16 h
  3. additionAnother 2 mL of AcOH was added to the mixture
  4. filtrationsolids were filtered off
  5. temperatureto warm up to rt
  6. customSolvent was evaporated
  7. customthe oily residue was purified by column chromatography (7.5% MeOH in dichloromethane)

出典と根拠

ORDレコード
ord-a8687c72c67c4ac58a83e6e9910ca957
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09273055B2

反応ノート

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