Triethylamine → N-(4-(2-((2,4-dichlorobenzyl)(methyl)amino)acetyl)phenyl)acetamide

HRID 45667

反応式

HRID 45667 の反応式
Br[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12](=[O:14])[CH3:13])=[CH:7][CH:6]=1)=[O:4].C(N(CC)CC)C.[Cl:22][C:23]1[CH:28]=[C:27]([Cl:29])[CH:26]=[CH:25][C:24]=1[CH2:30][NH:31][CH3:32]>O1CCOCC1>[Cl:22][C:23]1[CH:28]=[C:27]([Cl:29])[CH:26]=[CH:25][C:24]=1[CH2:30][N:31]([CH3:32])[CH2:2][C:3]([C:5]1[CH:10]=[CH:9][C:8]([NH:11][C:12](=[O:14])[CH3:13])=[CH:7][CH:6]=1)=[O:4]

参加物

5

反応物 3

HCID 8471TriethylamineHCID 485424Benzenemethanamine, 2,4-dichloro-N-methyl-HCID 12364739N-[4-(2-Bromoacetyl)Phenyl]Acetamide

生成物 1

HCID 12149183N-(4-(2-((2,4-dichlorobenzyl)(methyl)amino)acetyl)phenyl)acetamide収率 105%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

反応条件

温度
20 °C

実験手順

Into a 100-mL 3-necked round-bottom flask purged and maintained with an inert atmosphere of nitrogen, was placed a solution of N-(4-(2-bromoacetyl)phenyl)acetamide (1 g, 3.91 mmol, 1.00 equiv) in 1,4-dioxane (40 mL). This was followed by the addition of triethylamine (1.58 g, 15.64 mmol, 4.00 equiv) dropwise with stirring at 20° C. To this was added (2,4-dichlorophenyl)-N-methylmethanamine (880 mg, 4.63 mmol, 1.19 equiv) dropwise with stirring at 20° C. The resulting solution was stirred for 4 h at 20° C. The solids were filtered out. The resulting mixture was concentrated under vacuum to give 1.5 g (84%) of N-(4-(2-((2,4-dichlorobenzyl)(methyl)amino)acetyl)phenyl)acetamide as a white solid.

後処理

  1. customInto a 100-mL 3-necked round-bottom flask purged
  2. temperaturemaintained with an inert atmosphere of nitrogen
  3. stirringwith stirring at 20° C
  4. stirringThe resulting solution was stirred for 4 h at 20° C
  5. filtrationThe solids were filtered out
  6. concentrationThe resulting mixture was concentrated under vacuum

出典と根拠

ORDレコード
ord-a15f62929763400b923fba33a8d50f38
出典データセット
uspto-grants-2013_09
特許番号
US08541448B2

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