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Sodium Hydroxide → HCID 9933828, 화합물

HRID 1787213
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HRID 1787213 반응식
[Cl-].[Al+3].[Cl-].[Cl-].[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH:11]([C:14]1[CH:19]=[CH:18][C:17]([CH:20]2[C:24]3[C:25]([CH3:43])=[C:26]([NH:31][C:32](=O)[CH2:33][C:34]4[CH:39]=[CH:38][C:37]([O:40][CH3:41])=[CH:36][CH:35]=4)[C:27]([CH3:30])=[C:28]([CH3:29])[C:23]=3[O:22][C:21]2([CH3:45])[CH3:44])=[CH:16][CH:15]=1)([CH3:13])[CH3:12].[OH-].[Na+]>C1COCC1>[CH:11]([C:14]1[CH:15]=[CH:16][C:17]([CH:20]2[C:24]3[C:25]([CH3:43])=[C:26]([NH:31][CH2:32][CH2:33][C:34]4[CH:35]=[CH:36][C:37]([O:40][CH3:41])=[CH:38][CH:39]=4)[C:27]([CH3:30])=[C:28]([CH3:29])[C:23]=3[O:22][C:21]2([CH3:45])[CH3:44])=[CH:18][CH:19]=1)([CH3:13])[CH3:12]
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참가 물질

6

반응물 4

HCID 14798Sodium HydroxideHCID 6451240Aluminum(III) ChlorideHCID 10276991HCID 10276991, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 9933828HCID 9933828, 화합물수율 43%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran
용매

실험 절차

To a suspension of aluminum chloride (1.23 g, 9.25 mmol) in THF (40 mL) was slowly added lithium aluminium hydride (354 mg, 9.31 mmol) with ice-cooling, and the mixture was stirred at the same temperature for 10 minutes. To this mixture was added N-(3-(4-isopropylphenyl)-2,2,4,6,7-pentamethyl-2,3-dihydro-1-benzofuran-5-yl)-4-methoxyphenylacetamide obtained in Reference Example 365 (536 mg, 1.14 mmol), and the mixture was heated under reflux for 3 hours. The reaction mixture was added to ice-water, and the mixture was neutralized with a 8 N aqueous sodium hydroxide solution. Thereafter, the product was twice extracted with ethyl acetate, and the combined organic layer was washed with water, dried over magnesium sulfate, filtered and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1) to obtain 3-(4-isopropylphenyl)-N-(2-(4-methoxyphenyl)ethyl)-2,2,4,6,7-pentamethyl-2,3-dihydro-1-benzofuran-5-amine. This compound (537.9 mg, 1.18 mmol) was added to a suspension of sodium hydride (a 60% paraffin dispersion, 232.1 mg, 5.80 mmol) in DMF (25 mL) at 60° C., and the mixture was stirred for 20 minutes. Acetyl chloride (0.5 mL, 7.03 mmol) was added thereto, and the mixture was stirred at the same temperature for 1 hour. The reaction mixture was cooled to room temperature, and a saturated sodium hydrogen carbonate solution was added to the mixture, which was twice extracted with ethyl acetate. The extract was washed with water, dried over magnesium sulfate, filtered and then concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1) to obtain the rotational isomer of the object compound (Rf=0.38; hexane:ethyl acetate=3:1) (yield 43%). Melting point: 134-136° C. (ethyl acetate-hexane).

후처리

  1. temperaturecooling
  2. temperaturethe mixture was heated
  3. temperatureunder reflux for 3 hours
  4. extractionThereafter, the product was twice extracted with ethyl acetate
  5. washthe combined organic layer was washed with water
  6. dry with materialdried over magnesium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated under reduced pressure
  9. customThe residue was purified by silica gel column chromatography (hexane:ethyl acetate=3:1)

출처 및 근거

ORD 기록
ord-f9a20d0d047b4fa8ab2b22493c4b249d
출처 데이터셋
uspto-grants-2009_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07507841B2

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