Potassium Carbonate → HCID 22485267、化合物

HRID 353384

反応式

HRID 353384 の反応式
Cl.COC1C=C(C=CC=1OC)OC1C=CC(S([C:17]2(C(NO)=O)CC[N:20](CC#C)[CH2:19][CH2:18]2)(=O)=O)=CC=1.C([O-])([O-])=O.[K+].[K+].CO[C:43]1[CH:44]=[C:45](O)[CH:46]=[CH:47][C:48]=1[O:49]C>CN(C)C=O>[O:49]([NH:20][CH2:19][C:18]#[CH:17])[C:48]1[CH:43]=[CH:44][CH:45]=[CH:46][CH:47]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 162513,4-DimethoxyphenolHCID 1317238364-[[4-(3,4-dimethoxyphenoxy)phenyl] sulfonyl]-N-hydroxy-1-(2-propynyl)-4-piperidinecarboxamide, monohydrochloride

生成物 1

HCID 22485267HCID 22485267、化合物収率 90.9%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Part C: To a solution of the propargyl amine of part B (8 g, 22.63 mmol) and powdered K2CO3 (8.8 g, 56.6 mmol) in N,N-dimethylformamide (150 mL) was added 3,4-dimethoxyphenol (6.98 g, 45 mmol) at ambient temperature. The composition was heated to 90 degrees Celsius for 36 hours. The solution was concentrated under high vacuum and the residue was dissolved in ethyl acetate. The organic layer was washed with 1N NaOH, H2O and dried over MgSO4. Chromatography (on silica, ethyl acetate/hexane) provided phenoxy propargyl amine as light yellow gel (10 g, 90.9%).

後処理

  1. temperatureThe composition was heated to 90 degrees Celsius for 36 hours
  2. concentrationThe solution was concentrated under high vacuum
  3. dissolutionthe residue was dissolved in ethyl acetate
  4. washThe organic layer was washed with 1N NaOH, H2O
  5. dry with materialdried over MgSO4

出典と根拠

ORDレコード
ord-c4f247054abc48ff84edbe21d6b3c677
出典データセット
uspto-grants-2004_06
特許番号
US06750233B2

関連ノート

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