Pentane, 3-(bromomethyl)- → Dimethyl 5-(2-ethylbutoxyl)isophthalate

HRID 58991

反応式

HRID 58991 の反応式
[OH:1][C:2]1[CH:3]=[C:4]([C:12]([O:14][CH3:15])=[O:13])[CH:5]=[C:6]([CH:11]=1)[C:7]([O:9][CH3:10])=[O:8].Br[CH2:17][CH:18]([CH2:21][CH3:22])[CH2:19][CH3:20]>CC#N>[CH2:19]([CH:18]([CH2:21][CH3:22])[CH2:17][O:1][C:2]1[CH:11]=[C:6]([C:7]([O:9][CH3:10])=[O:8])[CH:5]=[C:4]([CH:3]=1)[C:12]([O:14][CH3:15])=[O:13])[CH3:20]

参加物

4

反応物 2

HCID 77432Pentane, 3-(bromomethyl)-HCID 830651,3-Benzenedicarboxylic acid, 5-hydroxy-, 1,3-dimethyl ester

生成物 1

HCID 117704493Dimethyl 5-(2-ethylbutoxyl)isophthalate

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

Dimethyl 5-hydroxyisophthalate (0.44 g, 2.10 mmol) cesium carbonate (1.37 g, 4.20 mmol) and CH3CN (20 mL) were added to a round-bottom flask and stirred for 15-30 min. 3-(Bromomethyl)pentane (0.42 g, 2.52 mmol) was added and the reaction was stirred for 16 h. The solvent was removed under reduced pressure and the reaction mixture was partitioned between EtOAc (50 mL) and H2O (50 mL). The layers were separated and the aqueous layer was extracted with EtOAc (50 mL). The combined organics were dried over Na2SO4, filtered, and concentrated under reduced pressure to afford the desired product which was used without further purification.

後処理

  1. stirringthe reaction was stirred for 16 h
  2. customThe solvent was removed under reduced pressure
  3. customthe reaction mixture was partitioned between EtOAc (50 mL) and H2O (50 mL)
  4. customThe layers were separated
  5. extractionthe aqueous layer was extracted with EtOAc (50 mL)
  6. dry with materialThe combined organics were dried over Na2SO4
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-70fc3e9a7f11415ca319a2dbe0c30442
出典データセット
uspto-grants-2016_09
特許番号
US09439433B2

関連ノート

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