Potassium Carbonate → HCID 86709754、化合物

HRID 1400292ノート

反応式

HRID 1400292 の反応式
[F:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][C:3]=1[OH:12].C([O-])([O-])=O.[K+].[K+].Br[CH2:20][CH2:21][NH:22][C:23](=[O:29])[O:24][C:25]([CH3:28])([CH3:27])[CH3:26].CCCCCC.C(OCC)(=O)C>CC(C)=O>[F:1][C:2]1[C:11]2[C:6](=[CH:7][CH:8]=[CH:9][CH:10]=2)[CH:5]=[CH:4][C:3]=1[O:12][CH2:20][CH2:21][NH:22][C:23](=[O:29])[O:24][C:25]([CH3:28])([CH3:27])[CH3:26]

参加物

6

反応物 4

HCID 11430Potassium CarbonateHCID 4103526tert-Butyl N-(2-bromoethyl)carbamateHCID 110949481-fluoronaphthalen-2-ol2 回HCID 21226206Ethyl acetate hexane

生成物 1

HCID 86709754HCID 86709754、化合物収率 65%

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

実験手順

To a solution of 1-fluoronaphthalen-2-ol (0.162 g, 1.0 mmol) and K2CO3 (0.300 g, 2.0 mmol) in acetone was added tert-butyl (2-bromoethyl)carbamate (0.336 g, 1.5 mmol). The resulting mixture was heated at reflux overnight. After TLC control (n-hexane/ethyl acetate 6:4) showed the disappearance of 1-fluoronaphthalen-2-ol, solvent was evaporated in vacuo and the residue was dissolved in 15 mL of ethyl acetate and washed with water (3×5 mL), brine (10 mL) and dried over Na2SO4. The evaporation of solvent afforded tert-butyl {2-[(1-fluoronaphthalen-2-yl)oxy]ethyl}carbamate as a white solid (65% yield) which was used without further purification.

後処理

  1. temperatureThe resulting mixture was heated
  2. temperatureat reflux overnight
  3. customwas evaporated in vacuo
  4. dissolutionthe residue was dissolved in 15 mL of ethyl acetate
  5. washwashed with water (3×5 mL), brine (10 mL)
  6. dry with materialdried over Na2SO4
  7. customThe evaporation of solvent

出典と根拠

ORDレコード
ord-060728d78dd34988bc3389efd60f68d4
出典データセット
uspto-grants-2014_12
特許番号
US08906946B2

反応ノート

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