Hydrochloric Acid → 1-{2-[1-(3,4-Dichlorophenyl)-5-methyl-1H-pyrazol-3-yloxy]ethyl}pyrrolidin-3-amine

HRID 220003ノート

反応式

HRID 220003 の反応式
[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13]([CH3:14])=[CH:12][C:11]([O:15][CH2:16][CH2:17][N:18]3[CH2:22][CH2:21][CH:20]([NH:23]C(=O)C)[CH2:19]3)=[N:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8].Cl.[OH-].[Na+]>O>[Cl:1][C:2]1[CH:3]=[C:4]([N:9]2[C:13]([CH3:14])=[CH:12][C:11]([O:15][CH2:16][CH2:17][N:18]3[CH2:22][CH2:21][CH:20]([NH2:23])[CH2:19]3)=[N:10]2)[CH:5]=[CH:6][C:7]=1[Cl:8]

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 57919736N-(1-(2-(1-(3,4-dichlorophenyl)-5-methyl-1H-pyrazol-3-yloxy)ethyl)pyrrolidin-3-yl)acetamide

生成物 1

HCID 115955611-{2-[1-(3,4-Dichlorophenyl)-5-methyl-1H-pyrazol-3-yloxy]ethyl}pyrrolidin-3-amine収率 90.1%

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

A solution of N-(1-(2-(1-(3,4-dichlorophenyl)-5-methyl-1H-pyrazol-3-yloxy)ethyl)pyrrolidin-3-yl)acetamide (0.1 g, 0.25 mmol) in water (2 ml) and 6N aqueous solution of HCl (2 ml) was refluxed for 5 hrs. The mixture was basified with 20% aqueous solution of NaOH and extracted with dichloromethane. The combined organic solutions was washed with water, dried over Na2SO4, filtered and evaporated to dryness yielding 80 mg of 1-{2-[1-(3,4-Dichlorophenyl)-5-methyl-1H-pyrazol-3-yloxy]ethyl}pyrrolidin-3-amine as an oil

後処理

  1. extractionextracted with dichloromethane
  2. washThe combined organic solutions was washed with water
  3. dry with materialdried over Na2SO4
  4. filtrationfiltered
  5. customevaporated to dryness

出典と根拠

ORDレコード
ord-9e7e6807a3144036a97a857a6c236417
出典データセット
uspto-grants-2012_06
特許番号
US08202872B2

反応ノート

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