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Sodium Hydroxide → HCID 68533199, 화합물

HRID 2108663
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HRID 2108663 반응식
[CH3:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]([CH3:31])[C:11]=1[CH2:12][C:13]1[CH:18]=[CH:17][C:16]([O:19][CH2:20][O:21][CH3:22])=[C:15]([CH2:23][C:24]2[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=2)[CH:14]=1)[C:5]([O:7]C)=[O:6].[OH-].[Na+]>CO>[CH3:1][C:2]1[CH:3]=[C:4]([CH:9]=[C:10]([CH3:31])[C:11]=1[CH2:12][C:13]1[CH:18]=[CH:17][C:16]([O:19][CH2:20][O:21][CH3:22])=[C:15]([CH2:23][C:24]2[CH:29]=[CH:28][C:27]([F:30])=[CH:26][CH:25]=2)[CH:14]=1)[C:5]([OH:7])=[O:6]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 14798Sodium HydroxideHCID 68529627HCID 68529627, 화합물2회

생성물 1

HCID 68533199HCID 68533199, 화합물수율 100%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
50 °C

실험 절차

To a stirring solution of afford methyl 3,5-dimethyl-4-[3′-(4-fluorobenzyl)-4′-methoxymethoxybenzyl]benzoate (compound 78, step f, 2.8 g, 6.63 mmol) in MeOH (80 mL) at 0° C. was added NaOH (27 mL, 1 N). After heating at 50° C. for 16 h, the solvent was removed under reduced pressure and the residue was acidified with 1 N HCl to pH=1, and the mixture was extracted with EtOAc. The organic layer was dried over Na2SO4, filtered and concentrated under reduced pressure to afford 3,5-dimethyl-4-[3′-(4-fluorobenzyl)-4′-methoxymethoxybenzyl]benzoic acid as white solid (2.7 g, 100%): 1H NMR (300 MHz, DMSO-d6): 12.71 (s, 1H), 7.64 (s, 2H), 7.01-7.22 (m, 4H), 6.95 (d, J=8.4 Hz, 1H), 6.85 (d, J=2.1 Hz, 1H), 6.73 (dd, J=2.1, 8.4 Hz, 1H), 5.15 (s, 2H), 3.98 (s, 2H), 3.86 (s, 2H), 3.27 (s, 3H), 2.25 (s, 6H).

후처리

  1. customthe solvent was removed under reduced pressure
  2. extractionthe mixture was extracted with EtOAc
  3. dry with materialThe organic layer was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-61d478ec8ad44f11a5616a7d3293de76
출처 데이터셋
uspto-grants-2009_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07514419B2

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