Potassium Carbonate → 3-(1,1-dimethyl-3-buten-1-yl)-4-methyl-5-phenyl-4H-1,2,4-triazole

HRID 550546ノート

反応式

HRID 550546 の反応式
[CH3:1][C:2]([CH3:10])([CH2:7][CH:8]=[CH2:9])[C:3]([NH:5][NH2:6])=O.C([O-])([O-])=O.[K+].[K+].Cl.[CH3:18][NH:19][C:20]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1)=NC>CN1C(=O)CCC1>[CH3:1][C:2]([C:3]1[N:19]([CH3:18])[C:20]([C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)=[N:6][N:5]=1)([CH3:10])[CH2:7][CH:8]=[CH2:9]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 12382386N,N'-dimethylbenzenecarboximidamide hydrochlorideHCID 576918522,2-Dimethyl-4-pentenohydrazide

生成物 1

HCID 576918753-(1,1-dimethyl-3-buten-1-yl)-4-methyl-5-phenyl-4H-1,2,4-triazole収率 32.1%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone溶媒

反応条件

温度
240 °C

実験手順

To a solution of 2,2-dimethyl-4-pentenohydrazide (360 mg) in NMP(2.5 ml) were added K2CO3 (348 mg) and N,N′-dimethylbenzenecarboximidamide hydrochloride (463 mmol). The solution was heated to the microwave at 240° C. for 30 minutes. Volatiles were evaporated in vacuo, the crude dissolved in DCM, washed with water and dried over Na2SO4. After filtration and concentration to dryness in vacuo, the crude was purified by column chromatography (DCM:MeOH=98 to 2) to give 196 mg of the title compound. MS (m/z): 242[MH]+.

後処理

  1. customVolatiles were evaporated in vacuo
  2. dissolutionthe crude dissolved in DCM
  3. washwashed with water
  4. dry with materialdried over Na2SO4
  5. filtrationAfter filtration and concentration to dryness in vacuo
  6. customthe crude was purified by column chromatography (DCM:MeOH=98 to 2)

出典と根拠

ORDレコード
ord-b5aa1ae7db544f1593f7c7c18c27cefc
出典データセット
uspto-grants-2011_05
特許番号
US07947683B2

反応ノート

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