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Sodium Hydroxide → 3-(2-Chloro-10,11-dihydro-dibenzo[b,f]oxepin-10-yl)-8-methyl-3,8-diazabicyclo(3.2.1)octane monomaleate

HRID 1274076
ノート
印刷プレビュー

反応式

HRID 1274076 の反応式
[Cl:1][C:2]1[CH:17]=[CH:16][C:5]2[O:6][C:7]3[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=3[CH:9](Cl)[CH2:10][C:4]=2[CH:3]=1.Cl.Cl.[CH3:20][N:21]1[CH:26]2[CH2:27][CH2:28][CH:22]1[CH2:23][NH:24][CH2:25]2.[C:29](=[O:32])([OH:31])[O-].[Na+].[OH-:34].[Na+]>CCOCC.CN(C)C=O>[C:5]([OH:34])(=[O:6])/[CH:4]=[CH:10]\[C:29]([OH:31])=[O:32].[Cl:1][C:2]1[CH:17]=[CH:16][C:5]2[O:6][C:7]3[CH:15]=[CH:14][CH:13]=[CH:12][C:8]=3[CH:9]([N:24]3[CH2:25][CH:26]4[N:21]([CH3:20])[CH:22]([CH2:28][CH2:27]4)[CH2:23]3)[CH2:10][C:4]=2[CH:3]=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

7

反応物 4

HCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 221201882,10-Dichloro-10,11-dihydro-dibenz[b,f]oxepinHCID 221201898-Methyl-3,8-diazabicyclo(3.2.1)octane dihydrochloride

生成物 1

HCID 867545003-(2-Chloro-10,11-dihydro-dibenzo[b,f]oxepin-10-yl)-8-methyl-3,8-diazabicyclo(3.2.1)octane monomaleate

試薬・触媒・溶媒 2

HCID 3283
Diethyl Ether
溶媒
HCID 6228Dimethylformamide溶媒

反応条件

温度
100 °C

実験手順

A mixture of 2,10-Dichloro-10,11-dihydro-dibenz[b,f]oxepin (3.2 g), 8-Methyl-3,8-diazabicyclo(3.2.1)octane dihydrochloride (1.6 g), sodium bicarbonate (10 g), and dimethylformamide (40 mL) was stirred at 100° C. for 1 h. After cooling, the reaction mixture was poured onto water, made basic with NaOH and the products are extracted with ether. The ether layer was extracted with 3N HCl, the aqueous layer is basified and the basic product was reextracted with ether. After drying over magnesium sulfate the solvent was removed in vacua. The residue is dissolved in ethanol and 500 mg of maleic acid was added and the mixture was warmed until a clear solution is obtained. After dilution of this mixture with ether and cooling at -20° C. overnight, 3-(2-Chloro-10,11-dihydro-dibenzo[b,f]oxepin-10-yl)-8-methyl-3,8-diazabicyclo(3.2.1)octane monomaleate (Compound 1) melting at 169-170° C. was obtained as white crystals.

後処理

  1. temperatureAfter cooling
  2. additionthe reaction mixture was poured onto water
  3. extractionthe products are extracted with ether
  4. extractionThe ether layer was extracted with 3N HCl
  5. dry with materialAfter drying over magnesium sulfate the solvent
  6. customwas removed in vacua
  7. dissolutionThe residue is dissolved in ethanol
  8. addition500 mg of maleic acid was added
  9. temperaturethe mixture was warmed until a clear solution
  10. customis obtained

出典と根拠

ORDレコード
ord-8172bec9b053490fbec03d37e81ed877
出典データセット
uspto-grants-2000_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06156751

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート