N,N-Dimethylethylenediamine → N-[2-(dimethylamino)ethyl]-4,5-diphenyl-1H-pyrazole-1-acetamide hemihydrate

HRID 1608289ノート

反応式

HRID 1608289 の反応式
[C:1]1([C:7]2[CH:8]=[N:9][N:10]([CH2:18][C:19]([O:21]CC)=[O:20])[C:11]=2[C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH3:24][N:25]([CH2:27][CH2:28][NH2:29])[CH3:26]>CCOCC>[OH2:20].[CH3:24][N:25]([CH3:26])[CH2:27][CH2:28][NH:29][C:19](=[O:21])[CH2:18][N:10]1[C:11]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[C:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[CH:8]=[N:9]1.[CH3:24][N:25]([CH2:27][CH2:28][NH:29][C:19](=[O:21])[CH2:18][N:10]1[C:11]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)=[C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[CH:8]=[N:9]1)[CH3:26]

参加物

4

反応物 2

HCID 66053N,N-Dimethylethylenediamine2 回HCID 146995514,5-Diphenyl-1-(ethoxycarbonylmethyl)-pyrazole

生成物 1

HCID 67948068N-[2-(dimethylamino)ethyl]-4,5-diphenyl-1H-pyrazole-1-acetamide hemihydrate収率 69.1%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

A mixture of 9 g (0.029 mol) of ethyl 4,5-diphenyl-1H-pyrazole-1-acetate of Example 1 and 31 mL (0.29 mol) of dimethylaminoethylamine was stirred on a steam bath under nitrogen for 18 hours. The excess dimethylamino ethylamine was stripped in vacuo, the residue dissolved in 300 mL of ether, treated with decolorizing carbon, filtered, and stripped to approximately 10 g of residue. This was triturated in water, filtered, washed and recrystallized from ether to yield 7.16 g of N-[2-(dimethylamino)ethyl]-4,5-diphenyl-1H-pyrazole-1-acetamide hemihydrate, mp 85°-88° C.

後処理

  1. additiontreated with decolorizing carbon
  2. filtrationfiltered
  3. customThis was triturated in water
  4. filtrationfiltered
  5. washwashed
  6. customrecrystallized from ether

出典と根拠

ORDレコード
ord-973509929b0748e29a6ff5777f89cc63
出典データセット
uspto-grants-1989_09
特許番号
US04870095

反応ノート

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