Potassium Carbonate → 9-(1-(4-Bromophenyl)ethyl)-4-cyclopropyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-one

HRID 1525862ノート

反応式

HRID 1525862 の反応式
Cl.[CH:2]1([N:5]2[CH2:10][C:9]3([CH2:15][CH2:14][NH:13][CH2:12][CH2:11]3)[O:8][CH2:7][C:6]2=[O:16])[CH2:4][CH2:3]1.C(=O)([O-])[O-].[K+].[K+].[Br:23][C:24]1[CH:29]=[CH:28][C:27]([CH:30](Br)[CH3:31])=[CH:26][CH:25]=1>CN(C)C=O.O>[Br:23][C:24]1[CH:29]=[CH:28][C:27]([CH:30]([N:13]2[CH2:12][CH2:11][C:9]3([O:8][CH2:7][C:6](=[O:16])[N:5]([CH:2]4[CH2:4][CH2:3]4)[CH2:10]3)[CH2:15][CH2:14]2)[CH3:31])=[CH:26][CH:25]=1

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 98381461-Bromo-4-(1-bromoethyl)benzeneHCID 69083351HCID 69083351、化合物

生成物 1

HCID 712708649-(1-(4-Bromophenyl)ethyl)-4-cyclopropyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-one

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A solution of 4-cyclopropyl-1-oxa-4,9-diazaspiro[5.5]undecan-3-one hydrochloride (0.341 mmol) in N,N-dimethylformamide (1.5 mL) was treated with potassium carbonate (0.682 mmol) and 1-bromo-4-(1-bromoethyl)benzene (0.341 mmol). The reaction mixture was stirred at room temperature overnight. The solution was diluted with water (50 mL) and was extracted three times with dichloromethane. The organic layers were combined, washed with brine, dried over sodium sulfate, filtered, and concentrated in vacuo to afford the title compound as a brown residue (117 mg, 87%). MS(ES)+ m/e 392.9/394.7 [M+H]+ (bromide isotope pattern).

後処理

  1. extractionwas extracted three times with dichloromethane
  2. washwashed with brine
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-9d72dd86c7e84953ab37b3b9a369ac35
出典データセット
uspto-grants-2015_07
特許番号
US09084794B2

反応ノート

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