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Lithium Hydroxide → HCID 59577007、化合物

HRID 2041978
ノート
印刷プレビュー

反応式

HRID 2041978 の反応式
[C:1]([C:5]1[CH:22]=[CH:21][CH:20]=[CH:19][C:6]=1[O:7][CH:8]1[CH2:11][N:10]([C:12](=[O:18])[C:13]([O:15]CC)=[O:14])[CH2:9]1)([CH3:4])([CH3:3])[CH3:2].[OH-].[Li+]>C(O)C>[C:1]([C:5]1[CH:22]=[CH:21][CH:20]=[CH:19][C:6]=1[O:7][CH:8]1[CH2:9][N:10]([C:12](=[O:18])[C:13]([OH:15])=[O:14])[CH2:11]1)([CH3:4])([CH3:2])[CH3:3]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 3939Lithium HydroxideHCID 59577194HCID 59577194、化合物

生成物 1

HCID 59577007HCID 59577007、化合物収率 65%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

反応条件

温度
0 °C

実験手順

To a stirred solution of ethyl 2-(3-(2-tert-butylphenoxy)azetidin-1-yl)-2-oxoacetate (1.65 g, 5.40 mmol) in ethanol (60.0 ml) was added lithium hydroxide (16.2 mL of 1.0 M solution in water, 16.2 mmol) at room temperature. After 1 h the reaction mixture was concentrated under reduced pressure, the resulting residue was diluted with water, cooled to 0° C., adjusted to about pH 1 with 1.0 N hydrochloric acid and the resulting solution was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride, dried (Na2SO4), filtered and concentrated under reduced pressure. The residue was recrystallized from heptane/ethyl acetate to provide 2-(3-(2-tert-butylphenoxy)azetidin-1-yl)-2-oxoacetic acid (0.97 g, 65%) as a white powder.

後処理

  1. concentrationAfter 1 h the reaction mixture was concentrated under reduced pressure
  2. additionthe resulting residue was diluted with water
  3. extractionthe resulting solution was extracted with ethyl acetate
  4. washThe organic layer was washed with saturated sodium chloride
  5. dry with materialdried (Na2SO4)
  6. filtrationfiltered
  7. concentrationconcentrated under reduced pressure
  8. customThe residue was recrystallized from heptane/ethyl acetate

出典と根拠

ORDレコード
ord-a5ad544785d34beb93db8da0dae66deb
出典データセット
uspto-grants-2013_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08586571B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート