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

HRID 553495ノート

反応式

HRID 553495 の反応式
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

参加物

5

反応物 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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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]+.

後処理

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

出典と根拠

ORDレコード
ord-73bd354241e04276b10e1492ec30aafe
出典データセット
uspto-grants-2011_11
特許番号
US08048884B2

反応ノート

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