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Ethyl chloroformate → (2-{5-[2-(5-Fluoro-2-methoxy-phenyl)-ethyl]-tetrahydro-furan-2-yl}-ethyl)-carbamic ethyl ester

HRID 1919540
ノート
印刷プレビュー

反応式

HRID 1919540 の反応式
C([O-])([O-])=O.[K+].[K+].Cl[C:8]([O:10][CH2:11][CH3:12])=[O:9].[NH2:13][CH2:14][CH2:15][CH:16]1[CH2:20][CH2:19][CH:18]([CH2:21][CH2:22][C:23]2[CH:28]=[C:27]([F:29])[CH:26]=[CH:25][C:24]=2[O:30][CH3:31])[O:17]1.C([O-])(O)=O.[Na+]>C1COCC1.CO.C(Cl)Cl>[CH2:11]([O:10][C:8](=[O:9])[NH:13][CH2:14][CH2:15][CH:16]1[CH2:20][CH2:19][CH:18]([CH2:21][CH2:22][C:23]2[CH:28]=[C:27]([F:29])[CH:26]=[CH:25][C:24]=2[O:30][CH3:31])[O:17]1)[CH3:12]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 10928Ethyl chloroformateHCID 11430Potassium CarbonateHCID 516892Sodium BicarbonateHCID 11587069Tetrahydrofuranyl ethylamine, 14

生成物 1

HCID 25258808(2-{5-[2-(5-Fluoro-2-methoxy-phenyl)-ethyl]-tetrahydro-furan-2-yl}-ethyl)-carbamic ethyl ester

試薬・触媒・溶媒 2

HCID 8028
Tetrahydrofuran
溶媒
2 回
HCID 21226129Dichloromethane methanol溶媒

反応条件

温度
0 °C

実験手順

Into a flame dried 20 mL vial was placed K2CO3 (239 mg, 1.73 mmol, 6.0 eq) and anhydrous THF (5.0 mL). The vial was purged with Ar(g) and then cooled in an ice bath. Ethyl chloroformate (156 mg, 1.44 mmol, 5.0 eq) was then added via syringe followed by slow addition of 14 (77 mg, 0.29 mmol, 1.0 eq) dissolved in THF (1.5 mL). The reaction was stirred at 0° C. for 0.5 hrs and then warmed to rt and allowed to stir an additional 3 hrs. The reaction was then stopped with sat. NaHCO3(aq) and extracted with EtOAc (3×20 mL). The organic layer was washed with brine and dried over Na2SO4, filtered, and concentrated under reduced pressure to yield crude product that was used in the next step of the synthesis. TLC: MeOH/CH2Cl2 (2:98, v:v), Rf 0.4; 1H NMR (CDCl3, 500 MHz) 6.87-6.82 (m, 2 H), 6.74-6.71 (m, 1 H), 4.12 (q, J=7.1 Hz, 2 H), 4.05-3.77 (m, 2 H), 3.78 (s, 3 H), 2.71-2.56 (m, 2 H), 2.08-1.51 (m, 10 H) 1.3 (t, J=7.2 Hz, 3 H). LRMS (ESI) [M+H]+ calcd for C18H27FNO4 340 found 340.

後処理

  1. customInto a flame dried 20 mL
  2. customThe vial was purged with Ar(g)
  3. temperaturecooled in an ice bath
  4. temperaturewarmed to rt
  5. stirringto stir an additional 3 hrs
  6. extractionextracted with EtOAc (3×20 mL)
  7. washThe organic layer was washed with brine
  8. dry with materialdried over Na2SO4
  9. filtrationfiltered
  10. concentrationconcentrated under reduced pressure
  11. customto yield crude product that
  12. customwas used in the next step of the synthesis

出典と根拠

ORDレコード
ord-0b4d62816ea646699435e35a6f951594
出典データセット
uspto-grants-2012_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08168635B2

反応ノート

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