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Sodium Hydroxide → 1-(Cyanomethyl)cyclobutane-1-carboxylic acid

HRID 920735
ノート
印刷プレビュー

反応式

HRID 920735 の反応式
[C:1]([CH2:3][C:4]1([C:8]([O:10]CC)=[O:9])[CH2:7][CH2:6][CH2:5]1)#[N:2].[OH-].[Na+]>C(O)C.C1COCC1.O>[C:1]([CH2:3][C:4]1([C:8]([OH:10])=[O:9])[CH2:7][CH2:6][CH2:5]1)#[N:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 2

HCID 14798Sodium HydroxideHCID 118061646Ethyl 1-(cyanomethyl)cyclobutanecarboxylate

生成物 1

HCID 1054280091-(Cyanomethyl)cyclobutane-1-carboxylic acid収率 66%

試薬・触媒・溶媒 3

HCID 702Ethanol溶媒HCID 962Water溶媒HCID 8028Tetrahydrofuran溶媒

実験手順

To a stirred solution of Intermediate 220B (0.110 g, 0.658 mmol) in ethanol (3.5 mL), THF (3.5 mL) and water (3 mL) was added NaOH (0.079 g, 1.974 mmol) and the reaction mixture was stirred at RT for 16 h. The reaction mixture was concentrated and the residue was diluted with water (3 mL) and extracted with EtOAc (3×20 mL) The pH of the aqueous layer was adjusted to 3 using a 1.5N aqueous solution of HCl and extracted with EtOAc (3×10 mL). The combined organic layer was washed with water, dried over Na2SO4, filtered and the filtrate concentrated. The residual mass was then azeotroped with toluene to obtain the Intermediate 220C as a brown oil (0.06 g, 66% yield). 1H NMR (400 MHz, DMSO-d6) δ ppm 12.65 (br. s., 1H), 3.04-2.79 (m, 2H), 2.42-2.17 (m, 2H), 2.09-1.67 (m, 4H).

後処理

  1. concentrationThe reaction mixture was concentrated
  2. additionthe residue was diluted with water (3 mL)
  3. extractionextracted with EtOAc (3×20 mL) The pH of the aqueous layer
  4. extractionextracted with EtOAc (3×10 mL)
  5. washThe combined organic layer was washed with water
  6. dry with materialdried over Na2SO4
  7. filtrationfiltered
  8. concentrationthe filtrate concentrated
  9. customThe residual mass was then azeotroped with toluene

出典と根拠

ORDレコード
ord-702d2d3feef943f3b6695821cc7c1321
出典データセット
uspto-grants-2016_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09273058B2

反応ノート

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