Potassium Hydroxide → HCID 13036368、化合物

HRID 128077ノート

反応式

HRID 128077 の反応式
C(OC([N:6]1[CH2:11][CH2:10][N:9]([C:12]2[N:13]=[C:14]3[CH:21]=[CH:20][CH:19]=[CH:18][CH:17]=[C:15]3[N:16]=2)[CH2:8][CH2:7]1)=O)C.[OH-].[K+]>C(O)C.O>[N:9]1([C:12]2[N:16]=[C:15]3[CH:17]=[CH:18][CH:19]=[CH:20][CH:21]=[C:14]3[N:13]=2)[CH2:10][CH2:11][NH:6][CH2:7][CH2:8]1

参加物

5

反応物 2

HCID 14797Potassium HydroxideHCID 13653113HCID 13653113、化合物

生成物 1

HCID 13036368HCID 13036368、化合物収率 126.2%

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

A mixture of 4-(2-cycloheptimidazolyl)-piperazine-1-carboxylic acid ethyl ester (2.86 g, described in Example 1) and potassium hydroxide in ethanol (20 ml) and water (1.5 ml) was refluxed for 20 hr. Water was added and the ethanol was evaporated. Additional water was added and the solution was extracted with chloroform. The organic extract was dried and evaporated to give the title compound (2.7 g). To a solution of the title compound in chloroform and diethyl ether, a solution of hydrogen chloride in diethyl ether was added. The precipitate was collected and crystallized from methanol-diethyl ether to obtain the hydrochloride salt of the title compound (2.4 g): mp>280° C.; ir(nujol) 2600, 1630 and 1584 cm-1 ; uv max (MeOH) 285(ε7540), 261(ε26,930) and 236 nm(ε18,310) and nmr(DMSO-d6)δ 3.37(4H,t), 4.3(4H,t), 8.4(5H,m) and 10.0(2H,s).

後処理

  1. temperaturewas refluxed for 20 hr
  2. customthe ethanol was evaporated
  3. additionAdditional water was added
  4. extractionthe solution was extracted with chloroform
  5. extractionThe organic extract
  6. customwas dried
  7. customevaporated

出典と根拠

ORDレコード
ord-e0c14630c92d4997a600a6aca555326e
出典データセット
uspto-grants-1981_03
特許番号
US04258188

反応ノート

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