Lithium hydroxide, monohydrate → 3-Methylsulfonyl-5-(2-oxopyrrolidin-1-yl)benzoic acid

HRID 1373107ノート

反応式

HRID 1373107 の反応式
[CH3:1][S:2]([C:5]1[CH:6]=[C:7]([CH:12]=[C:13]([N:15]2[CH2:19][CH2:18][CH2:17][C:16]2=[O:20])[CH:14]=1)[C:8]([O:10]C)=[O:9])(=[O:4])=[O:3].O.[OH-].[Li+]>O1CCOCC1.O>[CH3:1][S:2]([C:5]1[CH:6]=[C:7]([CH:12]=[C:13]([N:15]2[CH2:19][CH2:18][CH2:17][C:16]2=[O:20])[CH:14]=1)[C:8]([OH:10])=[O:9])(=[O:4])=[O:3]

参加物

5

反応物 2

HCID 168937Lithium hydroxide, monohydrateHCID 21074201Methyl 3-methylsulfonyl-5-(2-oxopyrrolidin-1-yl)-benzoate

生成物 1

HCID 210741993-Methylsulfonyl-5-(2-oxopyrrolidin-1-yl)benzoic acid

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 312751,4-Dioxane溶媒

実験手順

Methyl 3-methylsulfonyl-5-(2-oxopyrrolidin-1-yl)-benzoate (D18) (0.717 g) was suspended in dioxan (3.6 ml) and treated with a solution of lithium hydroxide monohydrate (0.153 g) in water (3.6 ml). The mixture was stirred for 2 h at room temperature and a clear solution was formed. The pH was adjusted to ˜4 by addition of Amberlyst-15 H+ resin. The resin was removed by filtration and washed well with dioxan. The combined filtrates were evaporated and the residue dried. Trituration with ether gave D19 (0.51 g) as a pale cream solid.

後処理

  1. customa clear solution was formed
  2. additionThe pH was adjusted to ˜4 by addition of Amberlyst-15 H+ resin
  3. customThe resin was removed by filtration
  4. washwashed well with dioxan
  5. customThe combined filtrates were evaporated
  6. customthe residue dried
  7. customTrituration with ether gave D19 (0.51 g) as a pale cream solid

出典と根拠

ORDレコード
ord-d95b5c951a5d4800a85ef027b5d38b9a
出典データセット
uspto-grants-2007_01
特許番号
US07160905B2

反応ノート

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