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

HRID 1356462ノート

反応式

HRID 1356462 の反応式
[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

参加物

5

反応物 3

HCID 66053N,N-DimethylethylenediamineHCID 18508368Methyl 4-(4-biphenylylmethoxy)phenylacetateHCID 178516071HCID 178516071、化合物

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-7c55b8e3a7dc4eae93244fc356c1ee9b
出典データセット
uspto-grants-2003_07
特許番号
US06586475B1

反応ノート

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