Water → 5-amino-3-(3-ethoxy-4-methoxyphenyl)-1-isopropyl-1H-pyrazole-4-carbonitrile

HRID 238063

反応式

HRID 238063 の反応式
[CH2:1]([O:3][C:4]1[CH:5]=[C:6]([C:12](OC)=[C:13]([C:16]#[N:17])[C:14]#[N:15])[CH:7]=[CH:8][C:9]=1OC)[CH3:2].Cl.[CH:21]([NH:24][NH2:25])([CH3:23])[CH3:22].[CH2:26](N(CC)CC)C.[OH2:33]>C(O)C>[NH2:15][C:14]1[N:24]([CH:21]([CH3:23])[CH3:22])[N:25]=[C:12]([C:6]2[CH:7]=[CH:8][C:9]([O:33][CH3:26])=[C:4]([O:3][CH2:1][CH3:2])[CH:5]=2)[C:13]=1[C:16]#[N:17]

参加物

6

反応物 4

HCID 962WaterHCID 8471TriethylamineHCID 855731-Isopropylhydrazine hydrochlorideHCID 866170192-((3-Ethoxy-4-methoxyphenyl)(methoxy)methylene)malononitrile

生成物 1

HCID 687116245-amino-3-(3-ethoxy-4-methoxyphenyl)-1-isopropyl-1H-pyrazole-4-carbonitrile

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

2-((3-ethoxy-4-methoxyphenyl)(methoxy)methylene)malononitrile (200 mg, 0.78 mmol), isopropylhydrazine hydrogen chloride (86 mg, 0.78 mmol), and triethylamine (0.10 mL, 0.78 mmol) were combined in ethanol (5 mL) and heated to reflux for 90 minutes. The reaction was then cooled to RT, water was added and the aqueous phase was extracted three times with EtOAc. The organic phase was concentrated and carried onto the next step without further characterization. ESI-MS (M+H)+ m/z calcd 301.1, found 301.0

後処理

  1. temperatureheated
  2. temperatureto reflux for 90 minutes
  3. extractionthe aqueous phase was extracted three times with EtOAc
  4. concentrationThe organic phase was concentrated

出典と根拠

ORDレコード
ord-00da41911aa64a5f8625edf0a235ac27
出典データセット
uspto-grants-2014_02
特許番号
US08642604B2

関連ノート

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