Hydrochloric Acid → N,N'-Dimethyl-N-(5-methyl-3-pyridyl)ethane-1,2-diamine dihydrochloride

HRID 631824ノート

反応式

HRID 631824 の反応式
[CH3:1][N:2]([CH2:10][CH2:11][N:12]([CH3:20])[C:13]1[CH:14]=[N:15][CH:16]=[C:17]([CH3:19])[CH:18]=1)C(=O)OC(C)(C)C.[ClH:21]>C(Cl)Cl>[ClH:21].[ClH:21].[CH3:20][N:12]([C:13]1[CH:14]=[N:15][CH:16]=[C:17]([CH3:19])[CH:18]=1)[CH2:11][CH2:10][NH:2][CH3:1]

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 131735429tert-Butyl N-methyl-N-[2-[methyl-(5-methyl-3-pyridyl)amino]ethyl]carbamate

生成物 1

HCID 89825869N,N'-Dimethyl-N-(5-methyl-3-pyridyl)ethane-1,2-diamine dihydrochloride

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

tert-Butyl N-methyl-N-[2-[methyl-(5-methyl-3-pyridyl)amino]ethyl]carbamate (301 mg, 1.078 mmol) was dissolved in DCM (40 ml). Hydrochloric acid (4M in dioxane, 5.4 ml) was added and the mixture was stirred at room temperature for 48 hours. The mixture was concentrated under reduced pressure, diethylether was added and the mixture was stirred at room temperature for 4 days. The solids were collected by filtration, rinsed with diethylether and dried under reduced pressure to yield 199 mg (0.789 mmol, 73%) MS(ESI) m/z=180.2 [M+1]+.

後処理

  1. concentrationThe mixture was concentrated under reduced pressure, diethylether
  2. additionwas added
  3. stirringthe mixture was stirred at room temperature for 4 days
  4. filtrationThe solids were collected by filtration
  5. washrinsed with diethylether
  6. customdried under reduced pressure
  7. customto yield 199 mg (0.789 mmol, 73%) MS(ESI) m/z=180.2 [M+1]+

出典と根拠

ORDレコード
ord-82ca38c6695d4dd8a0c6239fa6d85901
出典データセット
uspto-grants-2016_04
特許番号
US09321724B2

反応ノート

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