Hydrochloric Acid → {2-[4-(2-Chloro-pyridin-3-yl)-piperazin-1-yl]-ethyl}-methyl-amine hydrochloride salt

HRID 553495노트

반응식

HRID 553495 반응식
C(O[C:6](=O)[N:7]([CH2:9][CH2:10][N:11]1[CH2:16][CH2:15][N:14]([C:17]2[C:18]([Cl:23])=[N:19][CH:20]=[CH:21][CH:22]=2)[CH2:13][CH2:12]1)C)(C)(C)C.Cl.O1CCOCC1>ClCCl>[ClH:23].[Cl:23][C:18]1[C:17]([N:14]2[CH2:15][CH2:16][N:11]([CH2:10][CH2:9][NH:7][CH3:6])[CH2:12][CH2:13]2)=[CH:22][CH:21]=[CH:20][N:19]=1

참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 312751,4-DioxaneHCID 59252208{2-[4-(2-Chloro-pyridin-3-yl)-piperazin-1-yl]-ethyl}-methyl-carbamic acid tert-butyl ester

생성물 1

HCID 86640208{2-[4-(2-Chloro-pyridin-3-yl)-piperazin-1-yl]-ethyl}-methyl-amine hydrochloride salt수율 99%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

Dissolve {2-[4-(2-chloro-pyridin-3-yl)-piperazin-1-yl]-ethyl}-methyl-carbamic acid tert-butyl ester (4.900 g, 13.807 mmol) in dichloromethane (100 mL). Slowly add 4N HCl in dioxane (20.711 mL, 82.845 mmol). Stir at room temperature for 18 hr. Concentrate and wash the resulting solid with diethyl ether to afford the title preparation (7.500 g, 99% yield). MS ES: m/z=255 [M+H]+.

후처리

  1. concentrationConcentrate
  2. washwash the resulting solid with diethyl ether
  3. customto afford the title
  4. custompreparation (7.500 g, 99% yield)

출처 및 근거

ORD 기록
ord-73bd354241e04276b10e1492ec30aafe
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08048884B2

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