Potassium Carbonate → N-(2,4-difluorobenzyl)-N-heptyl-2-[4-(2-hydroxyethyl)-2-methoxyphenoxy]acetamide

HRID 898895ノート

反応式

HRID 898895 の反応式
Br[CH2:2][C:3]([N:5]([CH2:13][C:14]1[CH:19]=[CH:18][C:17]([F:20])=[CH:16][C:15]=1[F:21])[CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])=[O:4].[CH2:22]([OH:33])[CH2:23][C:24]1[CH:32]=[CH:31][C:29]([OH:30])=[C:26]([O:27][CH3:28])[CH:25]=1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C>[F:21][C:15]1[CH:16]=[C:17]([F:20])[CH:18]=[CH:19][C:14]=1[CH2:13][N:5]([CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])[C:3](=[O:4])[CH2:2][O:30][C:29]1[CH:31]=[CH:32][C:24]([CH2:23][CH2:22][OH:33])=[CH:25][C:26]=1[O:27][CH3:28]

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 16928Homovanillyl alcoholHCID 692602152-Bromo-N-(2,4-difluorobenzyl)-N-heptylacetamide

生成物 1

HCID 69258529N-(2,4-difluorobenzyl)-N-heptyl-2-[4-(2-hydroxyethyl)-2-methoxyphenoxy]acetamide収率 79%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

2-Bromo-N-(2,4-difluorobenzyl)-N-heptylacetamide (135 mg, 0.373 mmol), homovanillyl alcohol (63 mg, 0.373 mmol) and potassium carbonate anhydrous (77 mg, 0.559 mmol) were mixed in acetonitrile (10 ml). The mixture was heated to reflux for 4 hours and then evaporated to dryness. The residue (with additional DCM, 1 ml×2) was loaded onto a column (ISOLUTE® SI, 1 g/6 ml). It was eluted with DCM and then MeOH/DCM (0.5:99.5, then 1:99). The product fractions were combined and evaporated Oil product 132 mg was obtained yield 79%.

後処理

  1. temperatureThe mixture was heated
  2. temperatureto reflux for 4 hours
  3. customevaporated to dryness
  4. washIt was eluted with DCM
  5. customevaporated Oil product 132 mg
  6. customwas obtained yield 79%

出典と根拠

ORDレコード
ord-b130aecfd7b4448ea91286d0dd636d55
出典データセット
uspto-grants-2008_04
特許番号
US07351858B2

反応ノート

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