Potassium Hydroxide → HCID 13036368, 화합물

HRID 128077노트

반응식

HRID 128077 반응식
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

참가 물질

5

반응물 2

HCID 14797Potassium HydroxideHCID 13653113HCID 13653113, 화합물

생성물 1

HCID 13036368HCID 13036368, 화합물수율 126.2%

시약·촉매·용매 2

HCID 702Ethanol용매HCID 962Water용매2회

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-e0c14630c92d4997a600a6aca555326e
출처 데이터셋
uspto-grants-1981_03
특허 번호
US04258188

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