1H-1,2,4-Triazole → 4-(4-Biphenylylmethoxy)phenyl-N-[2-(N,N-dimethylamino)ethyl]acetamide

HRID 1356460노트

반응식

HRID 1356460 반응식
[C:1]1([C:20]2[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=2)[CH:6]=[CH:5][C:4]([CH2:7][O:8][C:9]2[CH:14]=[CH:13][C:12]([CH2:15][C:16](OC)=[O:17])=[CH:11][CH:10]=2)=[CH:3][CH:2]=1.[CH3:26][N:27]([CH3:31])[CH2:28][CH2:29][NH2:30].N1C=NC=N1>CO>[C:1]1([C:20]2[CH:21]=[CH:22][CH:23]=[CH:24][CH:25]=2)[CH:6]=[CH:5][C:4]([CH2:7][O:8][C:9]2[CH:14]=[CH:13][C:12]([CH2:15][C:16]([NH:30][CH2:29][CH2:28][N:27]([CH3:31])[CH3:26])=[O:17])=[CH:11][CH:10]=2)=[CH:3][CH:2]=1

참가 물질

5

반응물 3

HCID 92571H-1,2,4-TriazoleHCID 66053N,N-DimethylethylenediamineHCID 18508368Methyl 4-(4-biphenylylmethoxy)phenylacetate

생성물 1

HCID 99102684-(4-Biphenylylmethoxy)phenyl-N-[2-(N,N-dimethylamino)ethyl]acetamide수율 94.9%

시약·촉매·용매 1

HCID 887Methanol용매2회

반응 조건

온도
60 °C

실험 절차

A suspension of methyl 4-(4-biphenylylmethoxy)phenylacetate (1000 g), N,N-dimethylethylenediamine (795 g), and 1H-1,2,4-triazole (207 g) in methanol (2.0 l) was heated under reflux under nitrogen for 10 hr and was left to stand at room temperature over night. The reaction mixture was warmed to 60±2° C. and methanol (4.0 l) was added for 35 min. After stirring under reflux for additional one hr the reaction mixture was cooled to room temperature. The precipitate was collected by filtration and washed with methanol (2.0 l) to obtain the titled compound (1109 g).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux under nitrogen for 10 hr
  3. waitwas left
  4. waitto stand at room temperature over night
  5. temperatureunder reflux for additional one hr the reaction mixture
  6. temperaturewas cooled to room temperature
  7. filtrationThe precipitate was collected by filtration
  8. washwashed with methanol (2.0 l)

출처 및 근거

ORD 기록
ord-dca06a8293254f2abe4d91e1757cb4bb
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06586475B1

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