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Anisole → HCID 58452910, 화합물

HRID 70657
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HRID 70657 반응식
C1(OC)C=CC=CC=1.[C:9]([C:13]1[CH:18]=[CH:17][C:16](/[C:19](/[C:38]2[NH:43][C:42](=[O:44])[C:41]([CH2:45][CH3:46])=[CH:40][CH:39]=2)=[CH:20]\[C@H:21]2[CH2:25][CH2:24][C:23](=[O:26])[N:22]2CC2C=CC(OC)=CC=2OC)=[CH:15][CH:14]=1)([CH3:12])([CH3:11])[CH3:10]>FC(F)(F)C(O)=O>[C:9]([C:13]1[CH:14]=[CH:15][C:16](/[C:19](/[C:38]2[NH:43][C:42](=[O:44])[C:41]([CH2:45][CH3:46])=[CH:40][CH:39]=2)=[CH:20]\[C@H:21]2[CH2:25][CH2:24][C:23](=[O:26])[NH:22]2)=[CH:17][CH:18]=1)([CH3:12])([CH3:11])[CH3:10]
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참가 물질

4

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HCID 7519AnisoleHCID 674000826-{(E)-1-(4-tert-butylphenyl)-2-[(2R)-1-(2,4-dimethoxybenzyl)-5-oxopyrrolidin-2-yl]ethenyl}-3-ethylpyridin-2(1H)-one

생성물 1

HCID 58452910HCID 58452910, 화합물수율 57.6%

시약·촉매·용매 1

HCID 6422Trifluoroacetic acid용매2회

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온도
65 °C

실험 절차

Anisole (0.25 mL) was added to a solution of 6-{(E)-1-(4-tert-butylphenyl)-2-[(2R)-1-(2,4-dimethoxybenzyl)-5-oxopyrrolidin-2-yl]ethenyl}-3-ethylpyridin-2(1H)-one (49 mg) in trifluoroacetic acid (0.5 mL), and the mixture was stirred at 65° C. for seven hours. Trifluoroacetic acid (0.5 mL) was added and the mixture was stirred for further five hours, after which the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform:methanol=1:0→9:1). The resulting crystals (25 mg) were recrystallized from ethyl acetate-hexane to give the title compound as a colorless powder (20 mg).

후처리

  1. stirringthe mixture was stirred for further five hours
  2. customafter which the solvent was evaporated under reduced pressure
  3. customThe residue was purified by silica gel column chromatography (chloroform:methanol=1:0→9:1)
  4. customThe resulting crystals (25 mg) were recrystallized from ethyl acetate-hexane

출처 및 근거

ORD 기록
ord-f7673b04946f4042af1f379061569d09
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08822503B2

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