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Sodium Hydroxide → 1,2-Cyclopropanedicarboxylic acid, trans-

HRID 1504815
ノート
印刷プレビュー

反応式

HRID 1504815 の反応式
[OH-].[Na+].[C@@H:3]1([C:11]([O:13]CC)=[O:12])[CH2:5][C@H:4]1[C:6]([O:8]CC)=[O:7]>O.C(O)C>[C@@H:3]1([C:11]([OH:13])=[O:12])[CH2:5][C@H:4]1[C:6]([OH:8])=[O:7]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

HCID 14798Sodium HydroxideHCID 117153031,2-Diethyl (1R,2R)-1,2-cyclopropanedicarboxylate

生成物 1

HCID 69504501,2-Cyclopropanedicarboxylic acid, trans-

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒

実験手順

Sodium hydroxide (86.0 g, 2.15 mol) in water (400 mL) was added drop-wise to a stirred solution of diethyl rel-(1R,2R)-cyclopropane-1,2-dicarboxylate (200.0 g, 1.075 mol) in ethanol (400 mL) at 0° C. The reaction mixture was allowed to warm to ambient temperature. After 16 hours, the reaction mixture was concentrated under reduced pressure. The residue was diluted with cold water (500 mL) and extracted with ethyl acetate (2×500 mL). The organic layers were separated, and the aqueous layer was adjusted to pH˜2 using 1 N aqueous hydrochloric acid. The aqueous layer was extracted with ethyl acetate (2×1.0 L). The organic layers were combined, washed with water (1.0 L) and brine (500 mL), dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure to afford rel-(1R,2R)-cyclopropane-1,2-dicarboxylic acid. 1H NMR (400 MHz, DMSO-d6): δ 12.57 (s, 2H), 1.95-1.85 (m, 2H), 1.30-1.20 (m, 2H).

後処理

  1. concentrationthe reaction mixture was concentrated under reduced pressure
  2. additionThe residue was diluted with cold water (500 mL)
  3. extractionextracted with ethyl acetate (2×500 mL)
  4. customThe organic layers were separated
  5. extractionThe aqueous layer was extracted with ethyl acetate (2×1.0 L)
  6. washwashed with water (1.0 L) and brine (500 mL)
  7. dry with materialdried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-aea97f2d028f4263bdd592ee65444c50
出典データセット
uspto-grants-2015_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09216173B2

反応ノート

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