sym-Diethylurea → HCID 68828546、化合物

HRID 2099348ノート

反応式

HRID 2099348 の反応式
[CH:1]1([N:7]([C:23]([N:25]([CH2:28][CH3:29])[CH2:26][CH3:27])=[O:24])[CH:8]2[CH2:14][CH:13]3[N:15](C(OC(C)(C)C)=O)[CH:10]([CH2:11][CH2:12]3)[CH2:9]2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.C(NC(NCC)=O)C>Cl.C(OCC)C>[CH:10]12[NH:15][CH:13]([CH2:12][CH2:11]1)[CH2:14][CH:8]([N:7]([CH:1]1[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6]1)[C:23]([N:25]([CH2:26][CH3:27])[CH2:28][CH3:29])=[O:24])[CH2:9]2

参加物

5

反応物 2

HCID 12194sym-DiethylureaHCID 68828193HCID 68828193、化合物

生成物 1

HCID 68828546HCID 68828546、化合物

試薬・触媒・溶媒 2

HCID 313Hydrochloric Acid溶媒HCID 3283Diethyl Ether溶媒

実験手順

3.0 g of tert-butyl 3-{cyclohexyl[(diethyl-amino)carbonyl]amino}-8-azabicyclo[3.2.1]octane-8-carboxylate mixed with diethylurea are placed in 37 ml of 2N hydrochloric acid in diethyl ether. The reaction medium is stirred at ambient temperature for 16 h. After evaporation to dryness, the residue is taken up with a 1N aqueous hydrochloric acid solution. Extraction is carried out with ethyl acetate and a 1N aqueous sodium hydroxide solution is then added up to a pH of 10. Extraction is carried out with ethyl acetate until the aqueous phase is completely depleted. The organic phase is washed with H2O and then with a saturated aqueous sodium chloride solution. After drying over MgSO4 and concentration to dryness, 1.8 g of N-8-azabicyclo[3.2.1]oct-3-yl-N-cyclohexyl-N′,N′-diethylurea are obtained.

後処理

  1. customAfter evaporation to dryness
  2. extractionExtraction
  3. additiona 1N aqueous sodium hydroxide solution is then added up to a pH of 10
  4. extractionExtraction
  5. washThe organic phase is washed with H2O
  6. dry with materialAfter drying over MgSO4 and concentration to dryness, 1.8 g of N-8-azabicyclo[3.2.1]oct-3-yl-N-cyclohexyl-N′,N′-diethylurea
  7. customare obtained

出典と根拠

ORDレコード
ord-1a3f9abd8d394d0f84b4bd65bc3cdd3b
出典データセット
uspto-grants-2009_08
特許番号
US07569582B2

反応ノート

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