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

HRID 2073278노트

반응식

HRID 2073278 반응식
[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]

참가 물질

4

반응물 2

HCID 66053N,N-Dimethylethylenediamine2회HCID 146995514,5-Diphenyl-1-(ethoxycarbonylmethyl)-pyrazole

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-7b7cd5b27b8b4c8198959f82fc39bdb4
출처 데이터셋
uspto-grants-1990_04
특허 번호
US04916150

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