Hydrochloric Acid → 2-[2-(4-Phenylbutyl)phenoxymethyl]morpholine hydrochloride

HRID 743182노트

반응식

HRID 743182 반응식
C(OC([N:8]1[CH2:13][CH2:12][O:11][CH:10]([CH2:14][O:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH2:22][CH2:23][CH2:24][CH2:25][C:26]2[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=2)[CH2:9]1)=O)(C)(C)C.[ClH:32]>O1CCOCC1>[ClH:32].[C:26]1([CH2:25][CH2:24][CH2:23][CH2:22][C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=2[O:15][CH2:14][CH:10]2[O:11][CH2:12][CH2:13][NH:8][CH2:9]2)[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 106936854-t-Butoxycarbonyl-2-[2-(4-phenylbutyl)phenoxymethyl]morpholine

생성물 1

HCID 194240352-[2-(4-Phenylbutyl)phenoxymethyl]morpholine hydrochloride수율 86%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

671 mg of 4-t-butoxycarbonyl-2-[2-(4-phenylbutyl)phenoxymethyl]morpholine [prepared as described in step (a) above] was dissolved in 10 ml of a 4N solution of hydrogen chloride in dioxane, whilst ice-cooling, and the resulting solution was allowed to stand at room temperature for 30 minutes. At the end of this time, the solvent was removed by distillation under reduced pressure, and the resulting oily residue was dissolved in 20 ml of ethyl acetate. The solution thus obtained was then allowed to stand at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 494 mg (yield 86%) of the title compound as colorless crystals, melting at 131°-132° C.

후처리

  1. temperaturecooling
  2. customAt the end of this time, the solvent was removed by distillation under reduced pressure
  3. dissolutionthe resulting oily residue was dissolved in 20 ml of ethyl acetate
  4. customThe solution thus obtained
  5. customto stand at room temperature
  6. customThe crystals which precipitated
  7. filtrationwere collected by filtration
  8. customdried in vacuo

출처 및 근거

ORD 기록
ord-5d2dbb9ec4da44e5bf0a3741e7e0f4d6
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556864

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