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

HRID 1373107노트

반응식

HRID 1373107 반응식
[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]

참가 물질

5

반응물 2

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

생성물 1

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

시약·촉매·용매 2

HCID 962Water용매HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d95b5c951a5d4800a85ef027b5d38b9a
출처 데이터셋
uspto-grants-2007_01
특허 번호
US07160905B2

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