Hydrochloric Acid → HCID 86729431, 화합물

HRID 629520노트

반응식

HRID 629520 반응식
[C:1]12([C:11]3[CH:23]=[CH:22][C:14]([O:15][CH2:16][C:17]([O:19]CC)=[O:18])=[C:13]([CH3:24])[CH:12]=3)[CH2:10][CH:5]3[CH2:6][CH:7]([CH2:9][CH:3]([CH2:4]3)[CH2:2]1)[CH2:8]2.O.[OH-].[Li+].Cl>O.C1COCC1>[C:1]12([C:11]3[CH:23]=[CH:22][C:14]([O:15][CH2:16][C:17]([OH:19])=[O:18])=[C:13]([CH3:24])[CH:12]=3)[CH2:8][CH:7]3[CH2:9][CH:3]([CH2:4][CH:5]([CH2:6]3)[CH2:10]1)[CH2:2]2

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 168937Lithium hydroxide, monohydrateHCID 86729430HCID 86729430, 화합물

생성물 1

HCID 86729431HCID 86729431, 화합물수율 96.7%

시약·촉매·용매 1

HCID 21881883Oxolane--water (1/1)용매

실험 절차

To a solution of ethyl 2-(4-(adamantan-1-yl)-2-methylphenoxy)acetate (1.1 g, 3.50 mmol) in H2O/THF (1 mL/1.20 mL) was added lithium hydroxide monohydrate (0.29 g, 7.00 mmol), and stirred at room temperature overnight. The reaction mixture was adjusted to acidic solution with 1 N aqueous HCl and extracted with dichloromethane. The organic layer was washed with H2O and brine, and dried over anhydrous magnesium sulfate. The solvent was filtered and evaporated under reduced pressure to afford a crude solid, which was purified by silica gel column chromatography to give 2-(4-(adamantan-1-yl)-2-methylphenoxy)acetic acid as a white solid (0.54 g, 96.7% yield).

후처리

  1. extractionextracted with dichloromethane
  2. washThe organic layer was washed with H2O and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationThe solvent was filtered
  5. customevaporated under reduced pressure
  6. customto afford a crude solid, which
  7. customwas purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-13709abf4f8044078fa18887324c9429
출처 데이터셋
uspto-grants-2016_04
특허 번호
US09315507B2

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