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Hydrochloric Acid → HCID 20225207, 화합물

HRID 1249201
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HRID 1249201 반응식
Cl.[C:2]([CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH:15]([NH:17][CH2:18][CH:19]([O:27][CH3:28])[C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([Cl:26])[CH:21]=2)[CH3:16])=[CH:10][CH:9]=1)(OC)=[O:3].[CH3:29][NH2:30].Cl>CO.[Cl-].[Na+]>[ClH:26].[CH3:29][NH:30][C:2]([CH2:6][O:7][C:8]1[CH:13]=[CH:12][C:11]([CH2:14][CH:15]([NH:17][CH2:18][CH:19]([O:27][CH3:28])[C:20]2[CH:25]=[CH:24][CH:23]=[C:22]([Cl:26])[CH:21]=2)[CH3:16])=[CH:10][CH:9]=1)=[O:3]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 3

HCID 313Hydrochloric AcidHCID 6329Methylamine3회HCID 20225212HCID 20225212, 화합물

생성물 1

HCID 20225207HCID 20225207, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 5234Sodium Chloride용매

실험 절차

To a solution of N-[2-(4-carbomethoxymethoxyphenyl)-1-methylethyl]-2-methoxy-2-(3-chlorophenyl)ethanamine hydrochloride (0.63 g, diastereoisomeric ratio 92:8) in methanol was added 5 ml of a 30% aqueous solution of methylamine. This mixture was boiled under reflux for 6 hours during which time 3 further 5 ml portions of the methylamine solution were added. The solution was cooled to room temperature, a further 5 ml of methylamine solution added and the reaction mixture allowed to stand at room temperature overnight. After diluting with saturated sodium chloride solution the mixture was extracted with dichloromethane, washed with saturated sodium chloride solution, dried (magnesium sulphate), filtered and evaporated to give an oil which was converted to its hydrochloride salt by addition of ethereal hydrogen chloride. Recrystallisation from methanol-ethyl acetate gave the title compound, mp 217°-9° C., as single diastereoisomer.

후처리

  1. additionwere added
  2. extractionwas extracted with dichloromethane
  3. washwashed with saturated sodium chloride solution
  4. dry with materialdried (magnesium sulphate)
  5. filtrationfiltered
  6. customevaporated
  7. customto give an oil which
  8. customRecrystallisation from methanol-ethyl acetate

출처 및 근거

ORD 기록
ord-3a2237a7705d44a1b2938630a7c5200b
출처 데이터셋
uspto-grants-1986_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04629737

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