Hydrochloric Acid → 4-(2-{2-[2-(3-Hydroxyphenyl)ethyl]phenoxy}ethyl]-1-methylpiperidine hydrochloride

HRID 743280노트

반응식

HRID 743280 반응식
[ClH:1].COC[O:5][C:6]1[CH:7]=[C:8]([CH2:12][CH2:13][C:14]2[CH:29]=[CH:28][CH:27]=[CH:26][C:15]=2[O:16][CH2:17][CH2:18][CH:19]2[CH2:24][CH2:23][N:22]([CH3:25])[CH2:21][CH2:20]2)[CH:9]=[CH:10][CH:11]=1>O1CCOCC1>[ClH:1].[OH:5][C:6]1[CH:7]=[C:8]([CH2:12][CH2:13][C:14]2[CH:29]=[CH:28][CH:27]=[CH:26][C:15]=2[O:16][CH2:17][CH2:18][CH:19]2[CH2:24][CH2:23][N:22]([CH3:25])[CH2:21][CH2:20]2)[CH:9]=[CH:10][CH:11]=1

참가 물질

4

반응물 2

HCID 313Hydrochloric AcidHCID 194240154-(2-{2-[2-(3-Methoxymethoxyphenyl)ethyl]phenoxy}ethyl)-1-methylpiperidine

생성물 1

HCID 194238704-(2-{2-[2-(3-Hydroxyphenyl)ethyl]phenoxy}ethyl]-1-methylpiperidine hydrochloride수율 42%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매2회

실험 절차

2.3 ml of a 4N solution of hydrogen chloride in dioxane were added to a solution of 710 mg of 4-(2-{2-[2-(3-methoxymethoxyphenyl)ethyl]phenoxy}ethyl)-1-methylpiperidine [prepared as described in step (a) above] in 2.3 ml of dioxane, and the resulting mixture was allowed to stand at room temperature for 1 hour, after which it was concentrated by evaporation under reduced pressure. The resulting residue was dissolved in a small amount of methylene chloride, and ethyl acetate was added to the solution thus obtained, which was then allowed to stand at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 294 mg (yield 42%) of the title compound as a crystalline powder, melting at 130°-132° C.

후처리

  1. concentrationafter which it was concentrated by evaporation under reduced pressure
  2. dissolutionThe resulting residue was dissolved in a small amount of methylene chloride, and ethyl acetate
  3. additionwas added to the solution
  4. customthus 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-f8266d857baa47e69b36feab2ecbc9d5
출처 데이터셋
uspto-grants-1996_09
특허 번호
US05556864

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