Potassium Carbonate → HCID 86702008、化合物

HRID 717980ノート

反応式

HRID 717980 の反応式
[CH:1]1([C:4]#[C:5][C:6]([C:8]2[S:12][C:11]([C:13]([O:15][CH3:16])=[O:14])=[CH:10][CH:9]=2)=O)[CH2:3][CH2:2]1.Cl.[CH2:18]([NH:25][NH2:26])[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[CH2:18]([N:25]1[C:6]([C:8]2[S:12][C:11]([C:13]([O:15][CH3:16])=[O:14])=[CH:10][CH:9]=2)=[CH:5][C:4]([CH:1]2[CH2:3][CH2:2]2)=[N:26]1)[C:19]1[CH:24]=[CH:23][CH:22]=[CH:21][CH:20]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 14084Hydrazine, (phenylmethyl)-, hydrochloride (1:1)HCID 86702007HCID 86702007、化合物

生成物 1

HCID 86702008HCID 86702008、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

反応条件

温度
0 °C

実験手順

Methyl 5-(3-cyclopropylpropioloyl)thiophene-2-carboxylate (100 mg, 0.427 mmol) was dissolved in N,N-dimethylformamide (2 mL), and the solution was cooled to 0° C. Benzylhydrazine hydrochloride (74.5 mg, 0.470 mmol) was added followed by potassium carbonate (77 mg, 0.555 mmol). The mixture was stirred at 0° C. until the ice bath melted and was stirred overnight at room temperature. The solution was partitioned between water and ethyl acetate. The organic extract was dried with sodium sulfate, filtered, concentrated and purified by normal phase chromatography to afford the title compound.

後処理

  1. customThe solution was partitioned between water and ethyl acetate
  2. extractionThe organic extract
  3. dry with materialwas dried with sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated
  6. custompurified by normal phase chromatography

出典と根拠

ORDレコード
ord-fce876078c384025bb64a5b92df8c0a0
出典データセット
uspto-grants-2015_11
特許番号
US09193723B2

反応ノート

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