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Hydrochloric Acid → 6-(2-Hydroxy-4-methoxymethoxyphenyl)-5-hydroxymethyl-2,2,4-trimethyl-1,2-dihydroquinoline

HRID 1678272
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HRID 1678272 반응식
[H-].[Al+3].[Li+].[H-].[H-].[H-].[CH3:7][O:8][CH2:9][O:10][C:11]1[CH:12]=[C:13]2[C:26](=[CH:27][CH:28]=1)[C:25]1[C:16](=[C:17]3[C:22](=[CH:23][CH:24]=1)[NH:21][C:20]([CH3:30])([CH3:29])[CH:19]=[C:18]3[CH3:31])[C:15](=[O:32])[O:14]2.Cl>O1CCCC1.C(OCC)(=O)C.O>[OH:14][C:13]1[CH:12]=[C:11]([O:10][CH2:9][O:8][CH3:7])[CH:28]=[CH:27][C:26]=1[C:25]1[C:16]([CH2:15][OH:32])=[C:17]2[C:22](=[CH:23][CH:24]=1)[NH:21][C:20]([CH3:30])([CH3:29])[CH:19]=[C:18]2[CH3:31]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

7

반응물 3

HCID 313Hydrochloric AcidHCID 21226445Aluminium lithium hydrideHCID 579906038-Methoxymethoxy-2,2,4-trimethyl-1,2-dihydro-6-oxa-1-azachrysen-5-one

생성물 1

HCID 579906086-(2-Hydroxy-4-methoxymethoxyphenyl)-5-hydroxymethyl-2,2,4-trimethyl-1,2-dihydroquinoline

시약·촉매·용매 3

HCID 962Water용매
HCID 8028
Tetrahydrofuran
용매
2회
HCID 8857Ethyl Acetate용매2회

실험 절차

Lithium aluminum hydride (167 mg, 4.40 mmol) was suspended in anhydrous tetrahydrofuran (3 mL). A solution of 8-methoxymethoxy-2,2,4-trimethyl-1,2-dihydro-6-oxa-1-azachrysen-5-one (Reference Compound No. 1-(5), 744.1 mg, 2.12 mmol) in anhydrous tetrahydrofuran (10 mL) was added dropwise to the suspension at 0° C., the reaction mixture was stirred at the same temperature for 30 minutes. Ethyl acetate (2 mL) and water (1 mL) were added to the reaction mixture successively, and then ethyl acetate (150 mL) was added thereto. 1N aqueous HCl solution (6 mL) was added, the mixture was washed with water (100 mL, twice) and saturated brine (50 mL) successively, and then dried over anhydrous magnesium sulfate. The solvent was removed under reduced pressure to give the titled reference compound (750.6 mg) as a pale yellow amorphous product. (Quantitative)

후처리

  1. washthe mixture was washed with water (100 mL
  2. dry with materialtwice) and saturated brine (50 mL) successively, and then dried over anhydrous magnesium sulfate
  3. customThe solvent was removed under reduced pressure

출처 및 근거

ORD 기록
ord-7fb473753d0842f99f25672f3e2b4f26
출처 데이터셋
uspto-grants-2011_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08008497B2

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