Hydrochloric Acid → 2-Ethyl 3-[3-[4-(trifluoromethyl)benzylamino-methyl]-4-methoxyphenyl]propanoic acid hydrochloride

HRID 1826089노트

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HRID 1826089 반응식
[CH2:1]([CH:3]([CH2:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([CH2:18][NH:19][CH2:20][C:21]2[CH:26]=[CH:25][C:24]([C:27]([F:30])([F:29])[F:28])=[CH:23][CH:22]=2)[CH:11]=1)[C:4]([O:6]CC)=[O:5])[CH3:2].[OH-].[Na+].[ClH:33]>CO>[ClH:33].[CH2:1]([CH:3]([CH2:9][C:10]1[CH:15]=[CH:14][C:13]([O:16][CH3:17])=[C:12]([CH2:18][NH:19][CH2:20][C:21]2[CH:22]=[CH:23][C:24]([C:27]([F:28])([F:29])[F:30])=[CH:25][CH:26]=2)[CH:11]=1)[C:4]([OH:6])=[O:5])[CH3:2]

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 11122720Ethyl 2-ethyl-3-[3-[4-(trifluoromethyl)benzylaminomethyl]-4-methoxyphenyl]propanoate

생성물 1

HCID 865898562-Ethyl 3-[3-[4-(trifluoromethyl)benzylamino-methyl]-4-methoxyphenyl]propanoic acid hydrochloride수율 85%

시약·촉매·용매 1

HCID 887Methanol용매

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온도
60 °C

실험 절차

A mixture of ethyl 2-ethyl-3-[3-[4-(trifluoromethyl)benzylaminomethyl]-4-methoxyphenyl]propanoate (90.2 mg, 0.213 mmol), methanol (2 mL) and 2.5 mol/L aqueous solution of sodium hydroxide (2 mL) was stirred for 5 hours under heating at 60° C. After cooling, ice water (20 mL) was added and the mixture was made acidic with 1 mol/L hydrochloric acid, which was then saturated with sodium chloride and extracted with ethyl acetate. The extracte was washed with saturated brine, dried over anhydrous sodium sulfate, and then concentrated. The residue was purified by silica gel column chromatography (eluent: dichloromethane:methanol=10:1 v/v) to afford 78.0 mg (85%) of the title compound as a brown oil.

후처리

  1. temperatureAfter cooling
  2. extractionsaturated with sodium chloride and extracted with ethyl acetate
  3. washThe extracte was washed with saturated brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. concentrationconcentrated
  6. customThe residue was purified by silica gel column chromatography (eluent: dichloromethane:methanol=10:1 v/v)

출처 및 근거

ORD 기록
ord-30d74dc7e27b44578217ae3f4a319d93
출처 데이터셋
uspto-grants-2006_05
특허 번호
US07049342B2

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