Hydrochloric Acid → HCID 20186773, 화합물

HRID 2309009노트

반응식

HRID 2309009 반응식
[C:1]([CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][CH:14]([NH:16][CH2:17][CH:18]([O:26][CH2:27][CH2:28][OH:29])[C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([Cl:25])[CH:20]=2)[CH3:15])=[CH:9][CH:8]=1)(OC)=[O:2].[H-].[Al+3].[Li+].[H-].[H-].[H-].[OH-].[Na+].Cl>O1CCCC1.O>[ClH:25].[OH:2][CH2:1][CH2:5][O:6][C:7]1[CH:12]=[CH:11][C:10]([CH2:13][CH:14]([NH:16][CH2:17][CH:18]([O:26][CH2:27][CH2:28][OH:29])[C:19]2[CH:24]=[CH:23][CH:22]=[C:21]([Cl:25])[CH:20]=2)[CH3:15])=[CH:9][CH:8]=1

참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 21285459HCID 21285459, 화합물

생성물 1

HCID 20186773HCID 20186773, 화합물

시약·촉매·용매 2

HCID 962Water용매2회HCID 8028Tetrahydrofuran용매2회

실험 절차

N-[2-(4-Carbomethoxymethoxyphenyl)-1-methylethyl]-2-(2-hydroxyethoxy)-2-(3-chlorophenyl)ethanamine (3.0 g) in dry tetrahydrofuran (30 ml) was added dropwise, with stirring, to a suspension of lithium aluminium hydride (1.0 g) in dry tetrahydrofuran (30 ml) and the resultant mixture heated under reflux for 3 hours. After cooling, water (1 ml), 10% aqueous sodium hydroxide (1 ml) and water (2 ml) were added carefully. Filtration and evaporation of the filtrate to dryness gave an oil which was converted to its hydrochloride salt by treatment with ethereal hydrogen chloride. Recrystallisation from ethyl acetate-methanoldiethyl ether gave the title compound, mp 86°-90° C. as a 49:51 mixture of diastereoisomers.

후처리

  1. temperatureunder reflux for 3 hours
  2. temperatureAfter cooling
  3. filtrationFiltration and evaporation of the filtrate to dryness
  4. customgave an oil which
  5. customRecrystallisation from ethyl acetate-methanoldiethyl ether

출처 및 근거

ORD 기록
ord-1b32116c5d634e5dba2f33a89033212f
출처 데이터셋
uspto-grants-1987_09
특허 번호
US04692465

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