Lithium hydroxide, monohydrate → 2-(3-(Morpholin-4-yl)phenyl)acetic acid

HRID 1017566

反応式

HRID 1017566 の反応式
[N:1]1([C:7]2[CH:8]=[C:9]([CH2:13][C:14]([O:16]C)=[O:15])[CH:10]=[CH:11][CH:12]=2)[CH2:6][CH2:5][O:4][CH2:3][CH2:2]1.O.[OH-].[Li+]>CO.O>[N:1]1([C:7]2[CH:8]=[C:9]([CH2:13][C:14]([OH:16])=[O:15])[CH:10]=[CH:11][CH:12]=2)[CH2:2][CH2:3][O:4][CH2:5][CH2:6]1

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 18403524Methyl 3-(morpholin-4-yl)phenylacetate

生成物 1

HCID 184034952-(3-(Morpholin-4-yl)phenyl)acetic acid収率 90.4%

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 962Water溶媒

実験手順

To a solution of methyl 3-(morpholin-4-yl)phenylacetate (0.50 g, 2.1 mmol) in methanol (5 mL) and H2O (1 mL) was added lithium hydroxide monohydrate (0.18 g, 2 eq.). After the reaction mixture was stirred at room temperature overnight, it was concentrated to dryness. Acetic acid was then added to the residue and the resulting mixture was partitioned between EtOAc and H2O. The organic layer was washed with NaCl (sat.), dried over Na2SO4, and evaporation under vacuo to give 3-(morpholin-4-yl)phenylacetic acid (0.42 g).

後処理

  1. concentrationit was concentrated to dryness
  2. additionAcetic acid was then added to the residue
  3. customthe resulting mixture was partitioned between EtOAc and H2O
  4. washThe organic layer was washed with NaCl (sat.)
  5. dry with materialdried over Na2SO4, and evaporation under vacuo

出典と根拠

ORDレコード
ord-7f308cfca37b4e56b5b18d8b5d2b2669
出典データセット
uspto-grants-2002_11
特許番号
US06479490B2

関連ノート

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