Potassium Carbonate → HCID 2772320、化合物

HRID 2082131ノート

反応式

HRID 2082131 の反応式
[C:1]1(=[O:13])[NH:9][C:8](=[O:10])[CH:7]2[CH2:11][CH2:12][C:2]1([C:4]2([CH3:6])[CH3:5])[CH3:3].[Br-].[N:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[N:21]1[CH2:30][CH2:29][N+:24]2([CH2:28][CH2:27][CH2:26][CH2:25]2)[CH2:23][CH2:22]1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[N:15]1[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=1[N:21]1[CH2:22][CH2:23][N:24]([CH2:25][CH2:26][CH2:27][CH2:28][N:9]2[C:8](=[O:10])[CH:7]3[C:4]([CH3:6])([CH3:5])[C:2]([CH3:3])([CH2:12][CH2:11]3)[C:1]2=[O:13])[CH2:29][CH2:30]1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 160771,8,8-Trimethyl-3-azabicyclo[3.2.1]octane-2,4-dioneHCID 658423142348-17-2

生成物 1

HCID 2772320HCID 2772320、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 4.07 g (0.0225 mol) of DL-camphorimide (II), 6.71 g (0.0225 mol) of 8-(2-pyridyl)-8-aza-5-azoniaspiro[4,5]-decane bromide (III) and 3.73 g (0.027 mol) of potassium carbonate was refluxed in 80 ml of absolute dimethylformamide for 24 hours, then the resulting mixture was cooled, filtered, and dimethylformamide was distilled off under reduced pressure. The residue was dissolved in 100 ml of 5% HCl, the resulting solution was extracted twice with 50 ml of ether to remove impurities of non-basic nature, and saturated with soda. The precipitated base was extracted with ethyl acetate, the extract was dried with potassium carbonate and purified by passing through a column packed with a neutral aluminum oxide 5 cm thick (with ethyl acetate as eluent). After the solvent was distilled off, there was obtained a free base in the form of an oil which was then crystallized. Mp. 96°-97° C.

後処理

  1. temperaturethe resulting mixture was cooled
  2. filtrationfiltered
  3. distillationdimethylformamide was distilled off under reduced pressure
  4. dissolutionThe residue was dissolved in 100 ml of 5% HCl
  5. extractionthe resulting solution was extracted twice with 50 ml of ether
  6. customto remove impurities of non-basic nature
  7. extractionThe precipitated base was extracted with ethyl acetate
  8. dry with materialthe extract was dried with potassium carbonate
  9. custompurified
  10. distillationAfter the solvent was distilled off
  11. customthere was obtained a free base in the form of an oil which
  12. customwas then crystallized

出典と根拠

ORDレコード
ord-6f1f677bfa544e6b87dd1454ef34d75b
出典データセット
uspto-grants-1993_02
特許番号
US05187277

反応ノート

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