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Benzoic Acid → 4-Isopropylamino-1-(4-methoxypyrid-3-ylmethyl)piperidine monobenzoic acid salt

HRID 1181514
ノート
印刷プレビュー

反応式

HRID 1181514 の反応式
[CH:1]([NH:4][CH:5]1[CH2:10][CH2:9][N:8]([CH2:11][C:12]2[CH:13]=[N:14][CH:15]=[CH:16][C:17]=2[O:18][CH3:19])[CH2:7][CH2:6]1)([CH3:3])[CH3:2].[C:20]([OH:28])(=[O:27])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>CC(OC)(C)C>[C:20]([OH:28])(=[O:27])[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1.[CH:1]([NH:4][CH:5]1[CH2:6][CH2:7][N:8]([CH2:11][C:12]2[CH:13]=[N:14][CH:15]=[CH:16][C:17]=2[O:18][CH3:19])[CH2:9][CH2:10]1)([CH3:3])[CH3:2]
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

4

反応物 2

HCID 243Benzoic Acid2 回HCID 11651846N-isopropyl-1-((4-methoxypyridin-3-yl)methyl)piperidin-4-amine

生成物 1

HCID 674274674-Isopropylamino-1-(4-methoxypyrid-3-ylmethyl)piperidine monobenzoic acid salt収率 82%

試薬・触媒・溶媒 1

HCID 15413tert-Butyl methyl ether溶媒3 回

反応条件

温度
52.5 °C

実験手順

To a 1L reaction flask equipped with a mechanical stirrer and a nitrogen inlet was added 4-isopropylamino-1-(4-methoxypyrid-3-ylmethyl)piperidine (45.7 g, 0.174 mol) and 200 mL of MTBE. The resulting mixture was heated to 50-55° C. to dissolve the solid. To this solution was added a solution of benzoic acid (21.3 g, 0.174 mol) in 100 mL of MTBE at 50-55° C. (Note: Heat may be needed to dissolve the benzoic acid in MTBE). This mixture was stirred at 50-55° C. for 30 minutes and then stirred at room temperature for 16 hours. The resulting solid was filtered and washed with 50 mL of MTBE and then dried under vacuum at 40° C. for 16 hours to give 54.9 g of the title intermediate as a white solid (82% yield; ≧99% purity).

後処理

  1. customequipped with a mechanical stirrer and a nitrogen inlet
  2. dissolutionto dissolve the solid
  3. temperatureHeat may
  4. stirringstirred at room temperature for 16 hours
  5. filtrationThe resulting solid was filtered
  6. washwashed with 50 mL of MTBE
  7. customdried under vacuum at 40° C. for 16 hours

出典と根拠

ORDレコード
ord-a87c5e90bd2a4943ac0f24fbc8b26e85
出典データセット
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07285564B2

反応ノート

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