Lithium Hydroxide → 5-Hydoxyisophthalic acid

HRID 45740

반응식

HRID 45740 반응식
[OH:1][C:2]1[CH:3]=[C:4]([C:12]([O:14]C)=[O:13])[CH:5]=[C:6]([CH:11]=1)[C:7]([O:9]C)=[O:8].[OH-].[Li+]>C1COCC1>[OH:1][C:2]1[CH:3]=[C:4]([C:12]([OH:14])=[O:13])[CH:5]=[C:6]([CH:11]=1)[C:7]([OH:9])=[O:8]

참가 물질

4

반응물 2

HCID 3939Lithium HydroxideHCID 830651,3-Benzenedicarboxylic acid, 5-hydroxy-, 1,3-dimethyl ester

생성물 1

HCID 692575-Hydoxyisophthalic acid수율 58%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
40 °C

실험 절차

To dimethyl 5-hydroxyisophthalate (4.0 g, 19.03 mmol, 1.00 equiv) in THF (10 mL) was added lithium hydroxide (20 mL, 2M in water) and the resulting solution was stirred overnight at 40° C. The mixture concentrated under vacuum to remove the organic solvents and then the pH of the solution was adjusted to ˜2 with 6N hydrochloric acid. The resulting solids were collected by filtration and dried in a vacuum oven to afford 2.0 g (58%) of 5-hydroxyisophthalic acid as a white solid.

후처리

  1. concentrationThe mixture concentrated under vacuum
  2. customto remove the organic solvents
  3. filtrationThe resulting solids were collected by filtration
  4. customdried in a vacuum oven

출처 및 근거

ORD 기록
ord-6caa6e20c67a41f6b1ca7271b7a871a0
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541448B2

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