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Lithium Hydroxide → 6-chloro-7-(4-cyano-2-methylphenoxy)-2-(trifluoromethyl)-2H-chromene-3-carboxylic acid

HRID 855012
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HRID 855012 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][C:13]1[CH:18]=[CH:17][C:16](I)=[CH:15][C:14]=1[CH3:20])[O:8][CH:7]([C:21]([F:24])([F:23])[F:22])[C:6]([C:25]([O:27]CC)=[O:26])=[CH:5]2.[Cu][C:31]#[N:32].C(OCC)(=O)C.[OH-].[Li+]>CN(C)C=O.O1CCCC1.O.C(O)C>[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][C:11]=1[O:12][C:13]1[CH:18]=[CH:17][C:16]([C:31]#[N:32])=[CH:15][C:14]=1[CH3:20])[O:8][CH:7]([C:21]([F:24])([F:22])[F:23])[C:6]([C:25]([OH:27])=[O:26])=[CH:5]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

9

반응물 4

HCID 3939Lithium HydroxideHCID 8857Ethyl AcetateHCID 58935024ethyl 6-chloro-7-(2-methyl-4-iodophenoxy)-2-(trifluoromethyl)-2H-chromene-3-carboxylateHCID 178418546HCID 178418546, 화합물

생성물 1

HCID 114640046-chloro-7-(4-cyano-2-methylphenoxy)-2-(trifluoromethyl)-2H-chromene-3-carboxylic acid수율 27%

시약·촉매·용매 4

HCID 702Ethanol용매
HCID 962Water용매
HCID 6228Dimethylformamide용매
HCID 8028Tetrahydrofuran용매

실험 절차

A solution of 0.34 g (0.63 mmol) of Ethyl 6-chloro-7-(2-methyl-4-iodophenoxy)-2-(trifluoromethyl)-2H-chromene-3-carboxylate and 68 mg (0.76 mmol) of copper (I) cyanide in 4 mL of anhydrous dimethylformamide was stirred to 130° C. overnight. LC-MS indicated that the reaction was completed. After cooling to room temperature, the reaction was dumped into 100 mL of ethyl acetate. The organic solution was then washed with 30% aqueous ethylenediamine solution three times to remove cupper, then washed with with brine, and dried over anhydrous magnesium sulfate. After removing the volatiles, the residue was purified on silica gel column with 1:9 EtOAc/hexane. The obtained compound (0.14 g, 0.32 mmol) was dissolved in 3 mL of tetrahydrofuran. To the resulting solution was added a solution of 67.2 mg (1.6 mmol) of lithium hydroxide (LiOH.2H2O) in 3 mL of water, followed by addition of 3 mL of ethanol. The resulting solution was heated to 50° C. for one hr, then at rt for one hr. The volatiles were removed. The residue was diluted with water, and acidified at 0° C. with dilute hydrochloric acid to pH=1, and the product was extracted with ethyl acetate. The combined organic extracts were washed with birne, and dried over anhydrous magnesium sulfate. After removing the volatiles, the residue was purified on reverse phase HPLC. The product was obtained as white solid, 70 mg, purity=100%, yield=27%. 1H NMR (CDCl3/CD3OD/300 MHz) 7.66(s, 1H), 7.56(d, 1H), 7.46(dd, J=1.5, 8.4 Hz, 1H), 7.34(s, 1H), 6.80(d, J=8.4 Hz, 1H), 6.51(s, 1H), 5.66(q, J=6.9 Hz, 1H), 2.31(s, 3H); MS (ES+) 410 (M+1, 100); HRMS (ES−) m/z calcd for (M−1; C19H10ClF3NO4) 408.0245, found 408.0227.

후처리

  1. washThe organic solution was then washed with 30% aqueous ethylenediamine solution three times
  2. customto remove cupper
  3. washwashed with with brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customAfter removing the volatiles
  6. customthe residue was purified on silica gel column with 1:9 EtOAc/hexane
  7. temperatureThe resulting solution was heated to 50° C. for one hr
  8. customThe volatiles were removed
  9. additionThe residue was diluted with water
  10. customacidified at 0° C. with dilute hydrochloric acid to pH=1
  11. extractionthe product was extracted with ethyl acetate
  12. washThe combined organic extracts were washed with birne
  13. dry with materialdried over anhydrous magnesium sulfate
  14. customAfter removing the volatiles
  15. customthe residue was purified on reverse phase HPLC
  16. customThe product was obtained as white solid, 70 mg, purity=100%, yield=27%

출처 및 근거

ORD 기록
ord-1f303428d2274370a6fe2fa8640d171a
출처 데이터셋
uspto-grants-2007_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07259266B2

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