Hydrochloric Acid → 1,2-Cyclopropanedicarboxylic acid, trans-
反応式
C([O:3][C:4]([C@@H:6]1[CH2:8][C@H:7]1[C:9]([O:11]CC)=[O:10])=[O:5])C.Cl.[Na+].[Cl-]>[OH-].[Na+]>[C@@H:7]1([C:9]([OH:11])=[O:10])[CH2:8][C@H:6]1[C:4]([OH:5])=[O:3]参加物
5
反応条件
- 温度
- 22 °C
実験手順
Diethyl carboxylate 3 (16.9 g, 19.3 mmol) was dissolved in 170 ml of 2N NaOH and heated under reflux for 1 h. The solution was stirred for additional 18 h at 22° C. The solution was cooled, adjusted to pH 3 with 2N HCl, saturated with NaCl, and finally extracted with ethyl acetate (2×100 ml). The pooled extracts were dried (Na2SO4), evaporated to dryness, and the white residue was used for the next step without further purification (8.5 g, 79%); mp 175–176° C. 1H-NMR (D2O): δ 1.42 (m, 2H), 2.18 (m, 4H).
後処理
- temperatureheated
- temperatureunder reflux for 1 h
- temperatureThe solution was cooled
- extractionfinally extracted with ethyl acetate (2×100 ml)
- dry with materialThe pooled extracts were dried (Na2SO4)
- customevaporated to dryness
- customthe white residue was used for the next step without further purification (8.5 g, 79%)
出典と根拠
- ORDレコード
- ord-eafa451b143c4798beed215005a9e1bc
- 出典データセット
- uspto-grants-2007_06
- 特許番号
- US07235695B2
反応ノート
読み込み中…