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Potassium Hydroxide → 5-Aminosulfonyl-N-(1-azabicyclo[2.2.2]oct-3-yl)-2-methoxybenzamide Hydrochloride Hydrate

HRID 364634
ノート
印刷プレビュー

反応式

HRID 364634 の反応式
Cl.Cl.[NH2:3][CH:4]1[CH:9]2[CH2:10][CH2:11][N:6]([CH2:7][CH2:8]2)[CH2:5]1.[OH-].[K+].NC1C2CCN(CC2)C1.[CH3:23][O:24][C:25]1[CH:33]=[CH:32][C:31]([S:34](=[O:37])(=[O:36])[NH2:35])=[CH:30][C:26]=1[C:27]([Cl:29])=[O:28]>O.O1CCCC1>[OH2:24].[ClH:29].[NH2:35][S:34]([C:31]1[CH:32]=[CH:33][C:25]([O:24][CH3:23])=[C:26]([CH:30]=1)[C:27]([NH:3][CH:4]1[CH:9]2[CH2:10][CH2:11][N:6]([CH2:7][CH2:8]2)[CH2:5]1)=[O:28])(=[O:36])=[O:37]
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 14797Potassium HydroxideHCID 1042285-(Aminosulphonyl)-2-methoxybenzoyl chlorideHCID 1232383-AminoquinuclidineHCID 197853Quinuclidine, 3-amino-, dihydrochloride

生成物 1

HCID 202393685-Aminosulfonyl-N-(1-azabicyclo[2.2.2]oct-3-yl)-2-methoxybenzamide Hydrochloride Hydrate

試薬・触媒・溶媒 2

HCID 962
Water
溶媒
HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A solution of 3-aminoquinuclidine dihydrochloride (2.5 g, 0.0126 mole) in 25 ml of water was treated with approximately 5 g of KOH and the resultant slurry/solution taken to complete dryness on the rotary evaporator at 50°/35 mm. The dry residue was carefully extracted by repeated triturations with warm tetrahydrofuran until a total volume of 130 ml had been collected and dried over magnesium sulfate. This solution of 3-aminoquinuclidine base was treated with a solution of 2-methoxy-5-sulfamylbenzoyl chloride (2.92 g, 0.0117 mole) in 50 ml of dry tetrahydrofuran by dropwise addition under nitrogen. The resultant very turbid solution was refluxed gently for about 30 min, then freed of tetrahydrofuran by allowing it to evaporate. The residue was taken up in 90% ethanol containing a few drops of ethereal hydrogen chloride, filtered and chilled. The solid produced was then recrystallized again to yield 4.3 g (97%), m.p. 233°-234° C. NMR, MS, and IR were in support of the structure proposed.

後処理

  1. customthe resultant slurry/solution taken to complete dryness on the rotary evaporator at 50°/35 mm
  2. extractionThe dry residue was carefully extracted
  3. customhad been collected
  4. dry with materialdried over magnesium sulfate
  5. temperatureThe resultant very turbid solution was refluxed gently for about 30 min
  6. customto evaporate
  7. filtrationfiltered
  8. temperaturechilled
  9. customThe solid produced
  10. customwas then recrystallized again
  11. customto yield 4.3 g (97%), m.p. 233°-234° C

出典と根拠

ORDレコード
ord-ec7aeb374982460d9ec68512f9989070
出典データセット
uspto-grants-1986_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04605652

反応ノート

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