N,N-Dimethylethylenediamine → 4-(4-Biphenylylmethoxy)phenyl-N-[2-(N,N-dimethylamino)ethyl]acetamide

HRID 1356462노트

반응식

HRID 1356462 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].OC1C=CC=CN=1>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 66053N,N-DimethylethylenediamineHCID 18508368Methyl 4-(4-biphenylylmethoxy)phenylacetateHCID 178516071HCID 178516071, 화합물

생성물 1

HCID 99102684-(4-Biphenylylmethoxy)phenyl-N-[2-(N,N-dimethylamino)ethyl]acetamide수율 93.3%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

A suspension of methyl 4-(4-biphenylylmethoxy)phenylacetate (2.00 g), N,N-dimethylethylenediamine (1.60 g), 2-hydroxypyridine (573 mg) in methanol (4.0 ml) was heated under reflux under nitrogen for 16 hr and cooled until the temperature of the reaction mixture reached to 60±2° C., to which methanol (8.0 ml) was added. The reaction mixture was heated under reflux for additional one hr and cooled to room temperature. The precipitate was collected by filtration and washed with methanol (4.0 ml to obtain the titled compound (2.18 g).

후처리

  1. temperaturewas heated
  2. temperatureunder reflux under nitrogen for 16 hr
  3. temperaturecooled until the temperature of the reaction mixture
  4. additionwas added
  5. temperatureThe reaction mixture was heated
  6. temperatureunder reflux for additional one hr
  7. filtrationThe precipitate was collected by filtration
  8. washwashed with methanol (4.0 ml

출처 및 근거

ORD 기록
ord-7c55b8e3a7dc4eae93244fc356c1ee9b
출처 데이터셋
uspto-grants-2003_07
특허 번호
US06586475B1

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