Heptane → 1,2,2-Trimethyl-1,3-cyclopentanedicarboxylic acid

HRID 1484010

반응식

HRID 1484010 반응식
[C:1]([O:9][CH3:10])(=[O:8])/[CH:2]=[CH:3]/[C:4]([O:6][CH3:7])=[O:5].[C:11]([OH:24])(=[O:23])[C:12]1([CH2:22][CH2:21][CH:17]([C:18]([OH:20])=[O:19])[C:14]1([CH3:16])[CH3:15])[CH3:13].CCCCCCC>C(OCC)(=O)C>[C:1]([O:9][CH3:10])(=[O:8])/[CH:2]=[CH:3]/[C:4]([O:6][CH3:7])=[O:5].[C:11]([OH:24])(=[O:23])[C:12]1([CH2:22][CH2:21][CH:17]([C:18]([OH:20])=[O:19])[C:14]1([CH3:16])[CH3:15])[CH3:13].[C:1]([O:9][CH3:10])(=[O:8])/[CH:2]=[CH:3]/[C:4]([O:6][CH3:7])=[O:5].[C:11]([OH:24])(=[O:23])[C:12]1([CH2:22][CH2:21][CH:17]([C:18]([OH:20])=[O:19])[C:14]1([CH3:16])[CH3:15])[CH3:13]

참가 물질

7

반응물 3

HCID 8900HeptaneHCID 214911,2,2-Trimethyl-1,3-cyclopentanedicarboxylic acid3회HCID 637568Dimethyl Fumarate3회

생성물 3

HCID 214911,2,2-Trimethyl-1,3-cyclopentanedicarboxylic acidHCID 637568Dimethyl FumarateHCID 117762171Dimethyl fumarate (+)-camphoric acid

시약·촉매·용매 1

HCID 8857Ethyl Acetate용매

실험 절차

Cocrystals of dimethyl fumarate and (+)-camphoric acid were prepared as follows. 150 mg of dimethyl fumarate and 225 mg of (+)-camphoric acid were dissolved in 3 ml of ethyl acetate with stirring and gentle heating. The clear solution was cooled to room temperature, and 9 ml of heptane were added. The unstirred solution was allowed to stand for 24 hours. The starting concentrations of dimethyl fumarate and (+)-camphoric acid were chosen such that the thermodynamically stable solid phase at equilibrium is the cocrystal of dimethyl fumarate and (+)-camphoric acid. The crystalline material that formed was isolated by vacuum filtration, and dried to yield the dimethyl fumarate: (+)-camphoric acid (1:16, by NMR) cocrystal form 1 (112 mg).

후처리

  1. customThe crystalline material that formed
  2. customwas isolated by vacuum filtration
  3. customdried

출처 및 근거

ORD 기록
ord-c10884af3f2948cd802d5f3e298534c0
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09421182B2

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