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Water → (S)-a-Hydroxy-cyclobutanepropanoic acid

HRID 2185532
ノート
印刷プレビュー

反応式

HRID 2185532 の反応式
CC(C)([O-:4])C.[K+].O.CN(OC)[C:10](=[O:18])[C@@H:11]([OH:17])[CH2:12][CH:13]1[CH2:16][CH2:15][CH2:14]1>C1COCC1>[OH:17][C@@H:11]([CH2:12][CH:13]1[CH2:16][CH2:15][CH2:14]1)[C:10]([OH:18])=[O:4]
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 3

HCID 962WaterHCID 21341076N-Methyl-N-methoxy2-(S)-hydroxy-3-cyclobutyl PropanamideHCID 23665647Potassium tert-butoxide

生成物 1

HCID 21341063(S)-a-Hydroxy-cyclobutanepropanoic acid収率 85.3%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

A suspension of 33.66 g (0.3 mol) of potassium t-butoxide in 50 mL of THF was treated with 5.40 mL (0.3 mol) of H2O. The resulting mixture was treated with a solution of 11.48 g (0.061 mol) of N-methyl-N-methoxy 2-(S)-hydroxy-3-cyclobutyl propanamide (from Step C) in 20 mL of THF and stirred at rt for 20 h. The mixture was concentrated and the residue was partitioned between 300 mL of ether and 200 mL of H2O and the layers were separated. The pH of the aqueous layer was adjusted to 2 with concentrated HCl and extracted with 300 mL of EtOAc. The extract was washed with 100 mL of sat'd NaCl, dried over MgSO4 and concentrated to afford 7.50 g (85%) of the title compound: 1H NMR (500 MHz) δ1.66-1.76 (m, 2H), 1.78-1.98 (4H), 2.06-2.16 (m, 2H), 2.51-2.61 (m, 1H), 4.20 (dd, J=8.0,4.0, 1H).

後処理

  1. concentrationThe mixture was concentrated
  2. customthe residue was partitioned between 300 mL of ether and 200 mL of H2O
  3. customthe layers were separated
  4. extractionextracted with 300 mL of EtOAc
  5. washThe extract was washed with 100 mL of sat'd NaCl
  6. dry with materialdried over MgSO4
  7. concentrationconcentrated

出典と根拠

ORDレコード
ord-72ccdd47e2274fc687c558bf8e3f9585
出典データセット
uspto-grants-2002_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06399619B1

反応ノート

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