Potassium Carbonate → HCID 46867019、化合物

HRID 1689884ノート

反応式

HRID 1689884 の反応式
[C:1]([N:8]1[CH2:13][CH2:12][NH:11][CH2:10][CH2:9]1)([O:3][C:4]([CH3:7])([CH3:6])[CH3:5])=[O:2].C(=O)([O-])[O-].[K+].[K+].[CH3:20][C:21]1[O:25][N:24]=[C:23]([CH2:26]OS(C)(=O)=O)[CH:22]=1>CC#N.O>[C:4]([O:3][C:1]([N:8]1[CH2:9][CH2:10][N:11]([CH2:26][C:23]2[CH:22]=[C:21]([CH3:20])[O:25][N:24]=2)[CH2:12][CH2:13]1)=[O:2])([CH3:7])([CH3:6])[CH3:5]

参加物

6

反応物 3

HCID 11430Potassium CarbonateHCID 143452tert-Butyl piperazine-1-carboxylateHCID 57476926Methanesulfonic acid 5-methyl-isoxazol-3-ylmethyl ester

生成物 1

HCID 46867019HCID 46867019、化合物収率 89.1%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6342Acetonitrile溶媒

実験手順

To a solution of N—BOC-piperazine (300 mg) in MeCN (5 mL) was added potassium carbonate (289 mg) followed by methanesulfonic acid 5-methyl-isoxazol-3-ylmethyl ester (369 mg). The reaction mixture was heated to reflux for 24 h. After cooling the reaction mixture was diluted with water, extracted into ethyl acetate, dried (MgSO4) and the solvent was removed in vacuo to yield 4-(5-methyl-isoxazol-3-ylmethyl)-piperazine-1-carboxylic acid tert-butyl ester (404 mg).

後処理

  1. temperatureThe reaction mixture was heated
  2. temperatureto reflux for 24 h
  3. temperatureAfter cooling the reaction mixture
  4. extractionextracted into ethyl acetate
  5. dry with materialdried (MgSO4)
  6. customthe solvent was removed in vacuo

出典と根拠

ORDレコード
ord-bab7f3ee5a124b4aaa179b97b3e2225f
出典データセット
uspto-grants-2012_04
特許番号
US08153629B2

反応ノート

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